A strip of material for the delivery of an oral care active is disclosed. The strip of material includes a structural elastic-like film backing layer including a strainable network having a first region and a second region formed of substantially the same material composition, the first region providing a first, elastic-like resistive force to an applied axial elongation, and the second region providing a second distinctive resistive force to further applied axial elongation, thereby providing at least two stages of resistive forces in use; and an oral care composition disposed on the film, the oral care composition including an oral care active.
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1. A stretchable tooth whitening treatment product, comprising:
a) a stretchable elastic-like film backing layer, having a transverse axis and having an average thickness of from about 0.1 mil to about 5.0 mil, the film including a blend of:
i from about 50% to about 90%, by weight of the film, of high-density polyethylene; and
ii from about 10% to about 50%, by weight of the film, of linear low-density polyethylene; and
b) an oral care composition disposed on the film, the oral care composition including:
i from about 50% to about 99.9%, by weight of the composition, of an adhesive polymer; and
ii from about 0.1% to about 50%, by weight of the composition, of a teeth whitening active;
said film backing layer including a strainable network having a first region and a second region, the first region providing a first, elastic-like resistive force to an applied axial elongation, and the second region providing a second distinctive resistive force to further applied axial elongation, thereby providing at least two stages of resistive forces in use; and
wherein said film has a flexural stiffness of less than 4 grams/cm and a poisson lateral contraction less than 0.8 when said film is subjected to about 25% elongation, or a poisson lateral contraction less than about 1.0 when subjected to about 50% elongation;
wherein said second region includes a plurality of raised rib-like elements, said elements having a major axis which is substantially parallel to said transverse axis.
2. A stretchable tooth whitening treatment product according to
3. A stretchable tooth whitening treatment product according to
4. A stretchable tooth whitening treatment product according to
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The present disclosure relates to a strip of material for delivery of an oral care active and to methods for applying oral care actives to the desired region of a user's mouth. More particularly, the present disclosure relates to an extensible or stretchable strip of material and optionally a release liner. Such systems and methods can be used, for example, for whitening teeth.
Tooth whitening and other at-home and in-office oral care procedures have become popular in today's culture. In the office tooth bleaching generally involves several visits to the dentist and the use of a rubber dam to protect the patient's gums from the bleaching agents. Out of the office tooth bleaching generally involves the use of a device or tray which is made in the dental office to fit the patient's teeth. The device is reused, and therefore, must be sufficiently sturdy to endure repeat handling, cleaning, filling, installation, and wearing. Typically, a patient uses the device in time periods when social contact can be avoided.
Non-professional programs are also available to persons interested in whitening their teeth using commercial products available in stores. The commercial products often provide a kit which includes a generic appliance and a container of bleaching gel. The obvious appeal is the lower cost of the program. A major disadvantage of this generic “one size fits all” appliance is the greater void space between the interior walls of the appliance and the teeth versus a professionally fitted appliance. Hence, in order to insure intimate contact of the bleaching gel and the teeth surfaces, more bleaching gel is required. Furthermore, the poorer fit means a greater loss of bleaching gel onto the gums, into the oral cavity, and eventual ingestion. Since generic appliances are not fitted to the individual user, they are even more bulky in the mouth than the fitted appliances and thus they restrict social discourse during use.
A recognized consumer need is a low cost commercial oral care delivery system that is comfortable to wear that can deliver a sufficient amount of an oral care substance. In addition, a delivery system is needed which does not require extensive user placement manipulation to be certain of good contact for optimal delivery. Furthermore, what is needed is a non-bulky active containment means that will permit the wearer to use the system during social discourse without interfering with the wearer's speech or appearance. Also needed is a containment means that will protect oral care substance from erosion from contact with other oral surfaces and, or saliva.
To address the need, at least with regard to out of the office tooth whitening, whitening strips were developed. Exemplary strip delivery systems and methods of using the strips are disclosed in U.S. Pat. Nos. 6,551,579 B2 and 7,122,199 B2, both to Sagel et al. and assigned to The Procter & Gamble Company, the disclosure of which is incorporated herein by reference. However, there is still a need for improvement as the known strips do not easily provide for customization for different sized users. As such, also needed is a delivery system that is customizable in length, i.e. stretchable, to allow a user to cover the desired number of teeth, without the negative side effects that a user would experience with an elastic material, such as, a pulling force or creeping. Further, there is a need to provide even better and more secure fit for strip-like delivery systems and/or to provide the user with feedback associated with the fit of the device while being worn.
In one embodiment, a strip of material for the delivery of an oral care active is provided. The strip of material includes a structural elastic-like film backing layer including a strainable network having a first region and a second region formed of substantially the same material composition, the first region providing a first, elastic-like resistive force to an applied axial elongation, and the second region providing a second distinctive resistive force to further applied axial elongation, thereby providing at least two stages of resistive forces in use; and an oral care composition disposed on the film, the oral care composition including an oral care active.
In another embodiment, a stretchable tooth treatment product is provided. The stretchable tooth treatment product includes a structural elastic-like film backing layer, having an average thickness of from about 0.1 mil to about 5.0 mil, the film including: from about 50% to about 90%, by weight of the film, of high-density polyethylene; and from about 10% to about 50%, by weight of the film, of linear low-density polyethylene; and an oral care composition disposed on the film, the oral care composition including: from about 50% to about 99.9%, by weight of the composition, of an adhesive polymer; and from about 0.1% to about 50%, by weight of the composition, of an oral care active.
In another embodiment, a stretchable tooth treatment product is provided. The stretchable tooth treatment product includes a backing layer; and an oral care composition disposed on the backing layer, the oral care composition including an oral care active. The stretchable tooth treatment product exhibits a Young's Modulus of less than about 50 MPa, a strain at break of at least about 250%, and a strain at yield of at least about 30%.
In another embodiment, a method of delivering an oral care active to a plurality of adjacent teeth is provided. The method includes providing a strip of material having a backing layer and an oral care composition disposed on the backing layer, the oral care composition including an oral care active, the strip of material exhibiting a Young's Modulus of less than about 50 MPa, a strain at break of at least about 250%, and a strain at yield of at least about 30%; adjusting the size of the strip of material so that the strip is of a sufficient size to individually fit a wearer's plurality of adjacent teeth when placed against the teeth; and applying the strip of material to the plurality of adjacent teeth.
In another embodiment, a stretchable tooth treatment product is provided. The stretchable tooth treatment product includes a backing layer; and an oral care composition disposed on the backing layer, the oral care composition including an oral care active. The stretchable tooth treatment product exhibits a Young's Modulus of less than about 50 MPa, an initial peel force of greater than about 0.05 N, and less than about 0.05 g of material remaining after an initial peel test as measured according to a Strip Removal Test.
In yet another embodiment, a method of delivering an oral care active to a plurality of adjacent teeth is provided. The method includes providing a strip of material having a backing layer and an oral care composition disposed on the backing layer, the oral care composition including an oral care active, the strip of material exhibiting a Young's Modulus of less than about 50 MPa, an initial peel force of greater than about 0.05 N, and less than about 0.05 g of material remaining after an initial peel test as measured according to a Strip Removal Test; adjusting the size of the strip of material so that the strip is of a sufficient size to individually fit a wearer's plurality of adjacent teeth when placed against the teeth; and applying the strip of material to the plurality of adjacent teeth.
These and other features, aspects and advantages of specific embodiments will become evident to those skilled in the art from a reading of the present disclosure.
While the specification concludes with claims which particularly point out and distinctly claim the present invention, it is believed that the present invention will be better understood from the following description of preferred embodiments, taken in conjunction with the accompanying drawings, in which like reference numerals identify identical elements and wherein:
The abbreviation “cm”, as used herein, means centimeter. The abbreviation “mm”, as used herein, means millimeter.
As used herein, the term “necked backing layer”, refers to a backing layer for a strip of material which has been constricted in at least one dimension by applying a tensioning force in a direction that is perpendicular to the desired direction of neck-down.
As used herein, the term “percent neckdown”, refers to the ratio determined by measuring the difference between the un-necked dimension and the stabilized necked dimensions of the backing layer in the direction of necking, and then dividing that difference by the un-necked dimension of the backing layer, then multiplying by 100.
Strip of Material
The oral active delivery device may be referred to as a strip of material, a strip or any other suitable name. None of these terms, however, is intended to limit the delivery device to any particular size, shape, composition, material, number of layers, thickness or other characteristic. Rather, the term strip is intended to generally refer to a length of material used to deliver an oral care active to a portion of the user's mouth.
The strip may have a shape that is adapted to fit a user's teeth. The strip may be designed to cover any one or more teeth. For example, the strip may substantially cover the front side of at least a user's front four teeth and two canine teeth or may cover more or fewer teeth when used. By substantially, it is meant that at least half of the front tooth surface is covered. The strip may cover all of the front tooth surface and may also cover portions of the gums adjacent to the teeth. For tooth whitening strips, the strip will generally begin coverage at the point where the surface of the teeth intersect the gums and extend from there away from the gums to cover all or a portion of the individual tooth surfaces.
The strip may be foldable over the tips and onto the back sides of one or more of the teeth. In certain embodiments, the shape of the strip will allow for canine tips to not be covered. By folding over the tips it is meant that the strip covers or wraps around the front side of the tooth over the tip and onto the back side of the tooth. Depending upon the size of the strip, the entire back side of the tooth including the adjacent gum may be covered or only a portion of the back side of the tooth.
The shape of the strip may be any shape which allows it to fit the user and work for the desired purpose. For example, the strip may be substantially trapezoidal in shape. The term substantially trapezoidal is used to mean any shape having four general sides where there are two sides which are generally parallel. This may result from many shapes, including where one side is convex and the opposing side is concave. The arched shape may help to reduce bunching of the strip and allow the strip to lay smoother along the surfaces of the teeth. The strip may be substantially rectangular in shape. This is used generally to mean a shape with four sides which each of two sides are close to parallel. Parallel is used broadly to include when sides are arched, not straight, and generally not perpendicular. Alternatively, the strip may be of any shape such as round or oval. The strip may also be of a shape with any numbers of sides. The shape of the strip does not need to be symmetrical, but can be if desired.
Any of the sides or edges of the strip may be notched, stair stepped, or arched. By notched it is meant that there is a recess, indentation, or curve of some type. By stair stepped it is meant that the side is not straight and may contain one or more stair steps. The strip may also contain slits, cross-slits, holes, perforations, or any suitable formation that allows for the canines to protrude through or be avoided by the strip of material.
Each strip may include a fold line. The fold line is defined as the part of the strip where the tips of the teeth meet the strip when the strip is folded or wrapped over the tips. This line may be from the point where one recess, stair step, or notch on one side extends into the strip the farthest to where the other recess, stair step, or notch extends into the strip the farthest on the opposing side. The fold line will generally extend from one side of the strip to another parallel side and along the longer part of the strip. The fold line may be self adjusting depending upon the size and shape of the strip. With a trapezoidal shape strip, the fold line will be determined based upon the positioning of the strip on a user's teeth.
The strip may have rounded corners. “Rounded corners” is defined as not having any sharp angles or points. The size of the strip can be any suitable size and may be designed to address many different factors, including the number of teeth to be bleached, the size of the teeth, and personal preference of the wearer. In general, the length of the strip is from about 2 cm to about 12 cm, but can be from about 3 cm to about 10 cm, from about 4 cm to about 6 cm or any desired length. If the strip is stair stepped on the sides or trapezoidal shaped, the longer side of the strip of material may be from about 3 cm to about 12 cm, from about 3.1 to about 10 cm, from about 3.5 cm to about 8 cm, from about 4 cm to about 8 cm or any other suitable length. The shorter side may be from about 0.1 cm to about 12 cm, from about 0.5 cm to about 8 cm, from about 1 cm to about 5 cm, from about 1.5 cm to about 3 cm or any other suitable size. The width of the strip of material will also depend upon many factors, including whether or not the strip of material wraps completely around the teeth and covers part or all of the front and back surfaces of the tooth. The width can be any suitable measurement, but has been found to work well in certain embodiments when from about 0.5 cm to about 4 cm or from about 1 cm to about 2 cm.
One or more layers of the strip may comprise materials such as polymers, natural and synthetic wovens, non-wovens, foil, paper, rubber, and combinations thereof. The layers, if any, may include one or more materials. The strip may be substantially water impermeable, permeable and/or dissolvable. The strip may include any materials with the desired flexural rigidity and compatibility with the actives to be used. The materials may comprise a single polymer or a mixtures of polymers. Suitable polymers include, but are not limited to, polyethylene, polypropylene, polyvinylacetate, polyethyl-vinylacetate, polyethyl-vinyl alcohol, polyurethane, polyesters such as Mylar® manufactured by DuPont, fluoroplastics such as Teflon® manufactured by DuPont, biodegradable polymers, renewable polymers, and combinations thereof. The strip has been found to be especially suitable when less than about 1 mm thick, less than about 0.5 mm thick, and more from about 0.001 to about 0.3 mm thick although other thicknesses are possible.
Flexural stiffness is a material property that is a function of a combination of thickness, width, and material modulus of elasticity. The following is a test method for measuring the rigidity of the strip of material. It determines the resistance to flexure of a sample by using a strain gauge affixed to the end of a horizontal beam. The opposite end of the beam presses across a strip of the sample to force a portion of the strip into a vertical groove in a horizontal platform upon which the sample rests. A microammeter, wired to the strain gauge is calibrated in grams of deflection force. The rigidity of the sample is read directly from the microammeter and expressed as grams per centimeter of sample strip width. In one embodiment, the strip of material has a flexural stiffness of less than about 5 grams/cm as measured on a Handle-O-Meter, model #211-300, available from Thwing-Albert Instrument Co. of Philadelphia, Pa., as per test method ASTM D2923-95. The strip of material may have a flexural stiffness less than about 4 grams/cm, less than about 3 grams/cm, or from about 0.1 grams/cm to about 1 grams/cm. Generally, it is desired that the flexural stiffness of the material is substantially constant and does not significantly change during normal use. For example, it may be desirable that the strip not need to be hydrated for the strip to achieve the low flexural stiffness in the above-specified ranges.
This relatively low stiffness enables the strip to drape over the contoured surfaces of teeth with very little force being exerted. That is, conformity to the curvature of the wearer's mouth and gaps between adjacent teeth is maintained because there is little residual force within strip of material to cause it to return to its substantially flat shape. The flexibility of the strip enables the strip of material to contact adjoining soft tissue over an extended period of time without physical irritation. The strip does not require pressure forming it against the teeth.
The strip is held in place on a plurality of adjacent teeth at least partially by an adhesive composition discussed in more detail below. The viscosity and general tackiness of the adhesive composition cause the strip of material to be adhesively attached to a plurality of adjacent teeth without substantial slippage under the potential friction from the lips, tongue, and other soft tissue rubbing against the backing layer during mouth movements associated with talking, drinking, etc. However, this adhesion to the teeth is low enough to allow the strip to be easily removed by the wearer by peeling off the strip using one's finger or fingernail. The strip is easily removable from the surfaces of the teeth without the use of an instrument, a chemical solvent, or undue friction. Chemical solvents include any organic solvents commonly used in oral care products such as alcohol and other safe solvents such as water, which could be used to dilute the gelling agent. Undue friction is described as any type of rubbing with one's finger or a soft implement, such as cotton balls, swabs, or gauze pads.
A peel force of from about 1 gram to about 1500 grams for a 1.5 cm strip width (approximately 1000 grams/cm) is all that is required in certain embodiments. The peel force may be from about 5 grams to about 1250 grams or from about 10 grams to about 1000 grams. The low peel force is desired for consumer handling purposes. The low peel force may be made possible by a non-aggressive gel substance. This works especially well when the flexural stiffness of the strip is low. The adhesion of a stiffer strip would have to be greater in proportion to the strip stiffness in order to prevent the strip from returning to its flat condition and pulling away from the contoured surface of a plurality of teeth.
Referring now to the drawings, and more particularly to
As shown in
As shown in
The fold line 35 will usually be placed over the tips of a user's teeth enabling the strip to fold down onto both the front side and the back side of the user's teeth. The strip may be placed so that the user's two canine teeth are just outside of corners 36 and 37. The fourth side 34 may be located close to the bottom edge of the front side of a user's bottom set of front teeth. Alternatively if the strip is worn on the user's top set of teeth, the fourth side 34 may be placed along the top part of the front side of a user's top set of front teeth. The third side 33 may be along the back side of a user's teeth.
Embodiments 50, 60, and 70 are illustrated by
Backing Layer
As noted above, the strip may include one or more layers of the same or different materials. In certain embodiments, the strip includes a backing layer. The backing layer may serve as a protective barrier to prevent, substantially prevent or reduce the amount of saliva contacting the oral care substance and leaching and/or erosion of the substance from the surface of the teeth by the wearer's lips, tongue, and other soft tissue. For some uses, it may be desirable for the substance to act upon the surface of tooth over an extended period of time, from several minutes to several hours. Thus, influencing or controlling leaching and/or erosion may be desirable.
The backing layer may be formed by several of the film making processes known in the art. The backing layer may be a polyethylene made by a blown process or a cast process. Processes, such as extrusion and other processes are also feasible.
While the backing layer may be constructed from a number of different extensible materials as are known in the art, the backing layer, for performance and cost reasons, in one example, may be constructed of a structural elastic-like film (SELF) web. The term “web” herein refers to a sheet-like material comprising a single layer of material or a laminate of two or more layers. In other embodiments, additional formation means for deforming a backing layer into a three-dimensional structure may be used, for example, ring-rolling, “micro-SELF” and “rotary knife aperturing” (RKA).
Each of the four formation means disclosed herein are disclosed as comprising a pair of inter-meshing rolls, typically steel rolls having inter-engaging ridges or teeth and grooves. However, it is contemplated that other means for achieving formation can be utilized, such as the deforming roller and cord arrangement disclosed in US 2005/0140057 published Jun. 30, 2005. Therefore, all disclosure of a pair of rolls herein is considered equivalent to a roll and cord, and a claimed arrangement reciting two inter-meshing rolls is considered equivalent to an inter-meshing roll and cord where a cord functions as the ridges of a mating inter-engaging roll. In one embodiment, the pair of intermeshing rolls of the instant invention can be considered as equivalent to a roll and an inter-meshing element, wherein the inter-meshing element can be another roll, a cord, a plurality of cords, a belt, a pliable web, or straps. Likewise, while the disclosure of four formation means is illustrated herein, other known formation technologies, such as creping, necking/consolidation, corrugating, embossing, button break, hot pin punching, and the like may also be used. The formation processes known as ring-rolling, micro-SELF and RKA are further disclosed in U.S. Patent Publication No. 2008/0217809, which is hereby incorporated by reference herein.
The first formation means for deforming a backing layer in accordance with the present disclosure is a process commonly referred to as “SELF” or “SELF'ing” process.
The mass density of high-density polyethylene can range from about 0.93 to about 0.97 g/cm3. Although the density of HDPE is only marginally higher than that of LDPE, HDPE has little branching, giving it stronger intermolecular forces and tensile strength than LDPE. The difference in strength exceeds the difference in density, giving HDPE a higher specific strength. It is also harder and more opaque and can withstand somewhat higher temperatures (120° C./248° F. for short periods, 110° C./230° F. continuously). HDPE, unlike polypropylene, cannot withstand normally-required autoclaving conditions. The lack of branching is ensured by an appropriate choice of catalyst (e.g., Ziegler-Natta catalysts) and reaction conditions. HDPE contains the chemical elements carbon and hydrogen.
LDPE is defined by a density range of from about 0.910 to about 0.940 g/cm3. It is not reactive at room temperatures, except by strong oxidizing agents, and some solvents cause swelling. It can withstand temperatures of 80° C. continuously and 95° C. for a short time. Made in translucent or opaque variations, it is quite flexible, and tough but breakable. LDPE has more branching (on about 2% of the carbon atoms) than HDPE, so its intermolecular forces (instantaneous-dipole induced-dipole attraction) are weaker, its tensile strength is lower, and its resilience is higher. Also, since its molecules are less tightly packed and less crystalline because of the side branches, its density is lower. LDPE contains the chemical elements carbon and hydrogen.
LLDPE is a substantially linear polymer (polyethylene), with significant numbers of short branches, commonly made by copolymerization of ethylene with longer-chain olefins. LLDPE differs structurally from conventional LDPE because of the absence of long chain branching. The linearity of LLDPE results from the different manufacturing processes of LLDPE and LDPE. In general, LLDPE is produced at lower temperatures and pressures by copolymerization of ethylene and such higher alpha-olefins as butene, hexene, or octene. The copolymerization process produces an LLDPE polymer that has a narrower molecular weight distribution than conventional LDPE and in combination with the linear structure, significantly different rheological properties.
In another embodiment, the web may comprise an extensible polymer at a temperature of from about 0 degrees C. to about 50 degrees C. Extensible polymers include, but are not limited to, polymeric materials that have a percent elongation/strain at break higher than about 50% in the machine direction, and in another embodiment, to having a percent elongation/strain at break higher than about 100% and a Young's Modulus less than about 2,500 MPa in the machine direction, in yet another embodiment, having a percent elongation/strain at break higher than about 100% and a Young's Modulus less than about 2,000 MPa in the machine direction, in yet another embodiment, having a percent elongation/strain at break higher than about 100% and a Young's Modulus less than about 1,000 MPa in the machine direction, and in yet another embodiment, having a percent elongation/strain at break higher than about 100% and a Young's Modulus less than about 500 MPa in the machine direction.
The percent elongation/strain at break is the amount of stretch the film underwent before the point of break. Young's Modulus and percent elongation/strain at break can be measured on a tensile test machine using ASTM standard test method D 882—Tensile
Testing of Thin Plastic Sheeting.
Examples of backing layer compositions according to the present disclosure are shown in Table 1.
TABLE 1
Backing Layer Compositions (weight percent)
Young's
Example
HDPE
LLDPE
Thickness
Modulus*
No.
Grade
(%)
Grade
(%)
(mil)
(MPa)
Strain @ Break %
1
Equistar
90
Exxon
10
0.35
1494
154
L5005
L1001.32
2
Equistar
90
LyondellBasell
10
1.10
495
458
L5005
GA501022
3
Equistar
90
LyondellBasell
10
0.70
587
345
L5005
GA501023
4
Equistar
90
LyondellBasell
10
0.35
981
251
L5005
GA501024
5
Equistar
80
LyondellBasell
20
1.10
397
478
L5005
GA501025
6
Equistar
80
LyondellBasell
20
0.70
486
385
L5005
GA501026
7
Equistar
80
LyondellBasell
20
0.35
688
254
L5005
GA501027
8
Equistar
70
LyondellBasell
30
1.10
362
485
L5005
GA501028
9
Equistar
70
LyondellBasell
30
0.7
381
365
L5005
GA501029
10
Equistar
70
LyondellBasell
30
0.35
654
255
L5005
GA501030
11
Equistar
60
LyondellBasell
40
0.7
377
404
L5005
GA501031
12
Equistar
60
LyondellBasell
40
0.35
544
254
L5005
GA501032
13
Equistar
50
LyondellBasell
50
0.7
280
415
L5005
GA501033
14
Equistar
50
LyondellBasell
50
0.35
460
249
L5005
GA501034
15
Equistar
70
Exxon
30
0.7
478
488
L5005
L3001.32
*Machine Direction
Referring to
SELF web 200 has a first surface and an opposing second surface. In one embodiment, as shown in
The first region 204 has an elastic modulus E1 and a cross-sectional area A1. The second region 206 has an elastic modulus E2 and a cross-sectional area A2.
In the illustrated embodiment, a portion of the SELF web 200 has been “formed” such that the SELF web 200 exhibits a resistive force along an axis, which in the case of the illustrated embodiment is substantially parallel to the longitudinal axis of the SELF web, when subjected to an applied axial elongation in a direction substantially parallel to the longitudinal axis. As used herein, the term “formed” refers to the creation of a desired structure or geometry upon the SELF web that will substantially retain the desired structure or geometry when it is not subjected to any externally applied elongations or forces, i.e. regions of formation. A SELF web of the present disclosure is comprised of at least a first region and a second region, wherein the first region is visually distinct from the second region. As used herein, the term “visually distinct” refers to features of the SELF web material which are readily discernible to the normal naked eye when the SELF web material or objects embodying these SELF web material are subjected to normal use.
Methods for forming SELF web materials include, but are not limited to, embossing by mating plates or rolls, thermoforming, high pressure hydraulic forming, or casting. While the entire portion of the SELF web 200 has been subjected to a forming operation, the present disclosure may also include subjecting to formation only a portion thereof, for example, a portion of a backing layer.
In one embodiment shown in
The rib-like elements 214 in the second region 216 may be separated from one another by unformed areas, essentially unembossed or debossed, or simply formed as spacing areas. In one embodiment, the rib-like elements 214 are adjacent one another and are separated by an unformed area of less than 0.10 inches as measured perpendicular to the major axis 216 of the rib-like element 214, and in one embodiment, the rib-like element 214 are contiguous having no unformed areas between them.
What makes the SELF web particularly well suited for use as a delivery system including a strip of material is that it exhibits a modified “Poisson lateral contraction effect” substantially less than that of an otherwise identical unformed base web of similar material composition. As used herein, the term “Poisson lateral contraction effect” describes the lateral contraction behavior of a backing material which is being subjected to an applied elongation. The Poisson's Lateral Contraction Effect (PLCE) is calculated using the following formula:
Where w2=The width of the sample under an applied longitudinal elongation
In one embodiment, the Poisson lateral contraction effect of the SELF web of the present disclosure is less than about 0.8 when the SELF web is subjected to about 25% elongation. In another embodiment, the SELF web exhibits a Poisson lateral contraction effect less than about 1.0 when the SELF web is subjected to about 50 or even 100% elongation. The Poisson lateral contraction effect of the strips of the present disclosure is determined by the amount of the web material which is occupied by the first and second regions, respectively. As the area of the SELF web material occupied by the first region increases, the Poisson lateral contraction effect also increases. Conversely, as the area of the SELF web material occupied by the second region increases the Poisson lateral contraction effect decreases. In one embodiment, the percent area of the SELF web material occupied by the first region is from about 2% to about 90%, and in another embodiment, from about 5% to about 50%.
Web materials of the prior art which have at least one layer of an elastomeric material will generally have a large Poisson lateral contraction effect, i.e., they will “neck down” as they elongate in response to an applied force. SELF web materials of the present disclosure can be designed to moderate if not substantially eliminate the Poisson lateral contraction effect.
For the SELF web 200, the direction of applied axial elongation, D, indicated by arrows 220 in
Referring now to
When the SELF web is subjected to an applied elongation, the SELF web exhibits an elastic-like behavior as it extends in the direction of applied elongation and returns to its substantially untensioned condition once the applied elongation is removed, unless the SELF web is extended beyond the point of yielding. The SELF web is able to undergo multiple cycles of applied elongation without losing its ability to substantially recover. Accordingly, the SELF web is able to return to its substantially untensioned condition once the applied elongation or force is removed.
While the SELF web may be easily and reversibly extended in the direction of applied axial elongation, in a direction substantially perpendicular to the first axis of the rib-like elements, the SELF web is not as easily extended in a direction substantially parallel to the first axis of the rib-like elements. The formation of the rib-like elements allows the rib-like elements to geometrically deform in a direction substantially perpendicular to the first or major axis of the rib-like elements, while requiring substantially molecular-level deformation to extend in a direction substantially parallel to the first axis of the rib-like elements.
The amount of applied force required to extend the SELF web is dependent upon the composition and cross-sectional area of the web material forming the SELF web and the width and spacing of the first regions, with narrower and more widely spaced first regions requiring lower applied extension forces to achieve the desired elongation. The first axis, (i.e., the length) of the first regions may be greater than the second axis, (i.e., the width) of the first region with a length to width ratio of from about 5:1 or greater.
In
TABLE 2
Young's Modulus*
Strain @ Yield
Example #15 from Table 1
(MPa)
(%)
Base Backing Layer (curve
478
28
710)
SELF Backing Layer
254
81
(curve 720)
*Machine Direction
The backing layer (Example #15 from Table 1) is SELF'd according to a process in which the toothed roll (the top roll) had teeth having a pitch of 0.060 inches, a tooth height of 0.075 inches, and a tooth spacing of 0.060 inches. The corners of the teeth were further rounded. The mating roll (bottom roll) was an un-toothed roll, that is, a roll having circumferentially extending ridges and grooves, similar to that shown in
This demonstrates that the SELF backing layer or web exhibits a lower Young's Modulus/higher Strain@Yield vs. the base backing layer or web, resulting in a backing layer that is easier to stretch while maintaining uniform deformation.
Additional comparisons of SELF'd backing layers vs. base backing layers according to the present disclosure are shown in Table 3:
TABLE 3
Examples of SELF'd Backing Layers vs. Base Backing Layers
Young's
Strain @
Strain @
Example
Modulus
Yield
Break
No.
Depth of
(MPa)
(%)
(%)
Example
From
Selfing
Engagement
Base
SELF'd
Base
SELF'd
Base
SELF'd
No.
Table 1
activation
(inch)
Film
Film
Film
Film
Film
Film
1
# 2
cd tooling,
0.045″
458
219
31
66
495
170
then rotating
2
# 2
cd tooling,
0.055″
458
232
31
87
495
102
then rotating
3
# 5
cd tooling,
0.045″
478
191
36
59
397
241
then rotating
4
# 5
cd tooling,
0.055″
478
188
36
100
397
133
then rotating
5
# 8
cd tooling,
0.055″
485
172
37
95
362
217
then rotating
6
# 3
cd tooling,
0.045″
345
264
98
139
587
147
then rotating
7
# 3
cd tooling,
0.055″
345
261
98
95
587
98
then rotating
8
# 9
cd tooling,
0.055″
365
201
97
134
381
139
then rotating
9
# 11
cd tooling,
0.055″
404
139
41
228
377
250
then rotating
10
# 13
cd tooling,
0.055″
415
146
45
262
280
265
then rotating
11
# 15
cd tooling,
0.045″
488
302
28
88
478
178
then rotating
12
# 15
md tooling
0.045″
488
230
28
78
478
290
For Example Nos. 1 to 11 in Table 3, the backing layers are cut layer in machine direction, rotated 90° and then SELF'd with according to a process in which the toothed roll (the top roll) had teeth having a pitch of 0.060 inches, a tooth height of 0.075 inches, and a tooth spacing of 0.060 inches. The corners of the teeth were further rounded. The mating roll (bottom roll) was an un-toothed roll, that is, a roll having circumferentially to extending ridges and grooves, similar to that shown in
For Example No. 12 in Table 3, the backing layers are cut layer in machine direction, rotated 90° and then SELF'd with according to a process in which the toothed roll (the top roll) had teeth having a pitch of 0.060 inches, a tooth height of 0.075 inches, and a tooth spacing of 0.060 inches. The corners of the teeth were further rounded. The mating roll (bottom roll) was an un-toothed roll, that is, a roll having circumferentially extending ridges and grooves, similar to that shown in
As can be seen from Table 3, the depth and frequency of rib-like elements can also be varied to control the available stretch of the SELF web. The available stretch is increased if for a given frequency of rib-like elements, the height or degree of deformation imparted on the rib-like elements is increased. Similarly, the available stretch is increased if for a given height or degree of deformation, the frequency of rib-like elements is increased.
Referring now to
Referring now to
In one embodiment, the method of formation can be accomplished in a static mode, where one discrete portion of a base film is deformed at a time. An example of such a method is shown in
The dynamic press of
Another method of forming the base material into a SELF web is vacuum forming. An example of a vacuum forming method is disclosed n commonly assigned U.S. Pat. No. 4,342,314, issued to Radel et al. on Aug. 3, 1982. Alternatively, the SELF web of the present disclosure may be hydraulically formed in accordance with the teachings of commonly assigned U.S. Pat. No. 4,609,518 issued to Curro et al. on Sep. 2, 1986. Each of the above said patents being incorporated herein by reference.
In
Alternatively, roll 504 may consist of a soft rubber. As the base film is passed between toothed roll 502 and rubber roll 504 the film is mechanically formed into the pattern provided by the toothed roll 502. The film within the grooved regions 508 will remain undeformed, while the film within the toothed regions 506 will be formed producing rib-like elements in the second regions.
Referring now to FIG, 18, there is shown an alternative apparatus generally indicated as 550 for forming the base film into a SELF web in accordance with the teachings of the present disclosure, Apparatus 550 includes a pair of rolls 552, 554. Rolls 552 and 554 each have a plurality of toothed regions 556 and grooved regions 558 extending about the circumference of rolls 552, 554 respectively, As the base film passes between rolls 552 and 554, the grooved regions 558 will leave portions of the film undeformed, while the portions of the film passing between toothed regions 556 will he formed producing rib-like elements in second regions 206. The embodiment of FIG, 18 is referred to as MD or machine direction SELFing because the web 200 can be stretched in MD direction.
Referring now to
The pair of rolls discussed above may include any number of teeth and grooves as desired. In addition, the teeth and grooves may be nonlinear, such as for example, curved, sinusoidal, zig-zag, etc. The size and amount of engagement of teeth and grooves may be of any desired dimensions. In one embodiment, the pitch of the teeth are from about 0.020 inches to about 0.180 inches; in another embodiment from about 0.030 inches to about 0.120 inches; in another embodiment from about 0.040 inches to about 0.100 to inches; and in yet another embodiment from about 0.050 inches to about 0.070 inches, or any individual value these ranges.
With reference to
As illustrated in
TABLE 4
Extensible strip
Dimension
Area
% area
Length
% length
Width
% width
(mm)
(mm2)
change
(mm)
change
(mm)
change
Non-stretched
15 × 76
1140
76
15
25% stretched
13.5 × 95
1282.5
12.50%
95
25%
13.5
−10.00%
50% stretched
12 × 114
1368
20.00%
114
50%
12
−20.00%
100% stretched
10 × 152
1520
33.33%
152
100%
10
−33.33%
TABLE 5
Extensible Strip
Distance btw.
Width of rib-
Height of rib-
rib-like
like elements
like elements
elements - center
(mm)
(mm)
to center (mm)
Non-stretched
0.36
1.31
1.63
25% stretched
0.85
1.29
1.45
50% stretched
1.26
1.22
1.27
100% stretched
1.89
1.02
0.96
For Tables 4 and 5, the measurements were made under an optical microscope.
Backing layer or web material may be comprised of polyolefins such as polyethylenes, including linear low density polyethylene (LLDPE), low density polyethylene (LDPE), ultra low density polyethylene (ULDPE), high density polyethylene (HDPE), or polypropylene and blends thereof with the above and other materials. Examples of other suitable polymeric materials which may also be used include, but are not limited to, polyester, polyurethanes, compostable or biodegradable polymers, heat shrink polymers, thermoplastic elastomers, metallocene catalyst-based polymers (e.g., INSITE® available from Dow Chemical Company and EXXACT® available from Exxon), and breathable polymers. The web materials may also be comprised of a synthetic woven, synthetic knit, nonwoven, apertured film, macroscopically expanded three-dimensional formed film, absorbent or fibrous absorbent material, foam filled composition or laminates and/or combinations thereof. The nonwovens may be made but not limited to any of the following methods: spunlace, spunbond, meltblown, carded and/or air-through or calender bonded, with a spunlace material with loosely bonded fibers being the preferred embodiment.
While the SELF web has been described as a single base layer of substantially planar polymeric film, other base materials or laminates of materials may also be used. Examples of base materials from which the SELF web can be made include two-dimensional apertured films and macroscopically expanded, three-dimensional, apertured formed films. Examples of macroscopically expanded, three-dimensional, apertured formed films are described in U.S. Pat. No. 3,929,135 issued to Thompson on Dec. 30, 1975; U.S. Pat. No. 4,324,246 issued to Mullane, et al. on Apr. 13, 1982; U.S. Pat. No. 4,342,314 issued to Radel, et al. on Aug. 3, 1982 U.S. Pat. No. 4,463,045 issued to Ahr, et al. on Jul. 31, 1984; and U.S. Pat. No. 5,006,394 issued to Baird on Apr. 9, 1991. Each of these patents are incorporated herein by reference. Examples of other suitable base materials include composite structures or laminates of polymer films, nonwovens, and polymer films and nonwovens. Additional reinforcing elements can also be added for strength and recovery benefits.
In another embodiment, the backing layer 812 may be an elastomeric nonwoven substrate or an elastomeric film that does not require selfing. Non-limiting examples of suitable elastomeric materials include thermoplastic elastomers chosen from at least one of styrenic block copolymers, metallocene-catalyzed polyolefins, polyesters, polyurethanes, polyether amides, and combinations thereof. Suitable styrenic block copolymers may be diblock, triblock, tetrablock, or other multi-block copolymers having at least one styrenic block. Example styrenic block copolymers include styrene-butadiene-styrene, styrene-isoprene-styrene, styrene-ethylene/butylenes-styrene, styrene-ethylene/propylene-styrene, and the like. Commercially available styrenic block copolymers include KRATON® from the Shell Chemical Company of Houston, Tex.; SEPTON® from Kuraray America, Inc. of New York, N.Y.; and VECTOR® from Dexco Polymers, LP of Houston, Tex. Commercially available metallocene-catalyzed polyolefins include EXXPOL® and EXACT® from Exxon Chemical Company of Baytown, Tex.; AFFINITY®; and ENGAGE® from Dow Chemical Company of Midland, Mich. Commercially available polyurethanes include ESTANE® from Noveon, Inc., Cleveland, Ohio. Commercial available polyether amides include PEBAX® from Atofina Chemicals of Philadelphia, Pa. Commercially available polyesters include HYTREL® from E. I. DuPont de Nemours Co., of Wilmington, Del. Other particularly suitable examples of elastomeric materials include elastomeric polypropylenes. In these materials, propylene represents the majority component of the polymeric backbone, and as a result, any residual crystallinity possesses the characteristics of polypropylene crystals. Residual crystalline entities embedded in the propylene-based elastomeric molecular network may function as physical crosslinks, providing polymeric chain anchoring capabilities that improve the mechanical properties of the elastic network, such as high recovery, low set and low force relaxation. Suitable examples of elastomeric polypropylenes include an elastic random poly(propylene/olefin) copolymer, an isotactic polypropylene containing stereoerrors, an isotactic/atactic polypropylene block copolymer, an isotactic polypropylene/random poly(propylene/olefin) copolymer block copolymer, a reactor blend polypropylene, a very low density polypropylene (or, equivalently, ultra low density polypropylene), a metallocene polypropylene, and combinations thereof. Suitable polypropylene polymers including crystalline isotactic blocks and amorphous atactic blocks are described, for example, in U.S. Pat. Nos. 6,559,262, 6,518,378, and 6,169,151. Suitable isotactic polypropylene with stereoerrors along the polymer chain are described in U.S. Pat. No. 6,555,643 and EP 1 256 594 A1. Suitable examples include elastomeric random copolymers (RCPs) including propylene to with a low level comonomer (e.g., ethylene or a higher α-olefin) incorporated into the backbone. Suitable elastomeric RCP materials are available under the names VISTAMAXX® (available from ExxonMobil, Houston, Tex.) and VERSIFY® (available from Dow Chemical, Midland, Mich.).
In another embodiment, the backing layer 812 may be formed by a process for selectively aperturing a nonwoven web. In one embodiment, the nonwoven web may be extensible, elastic, or nonelastic. The nonwoven web may be a spunbonded web, a meltblown web, or a bonded carded web. If the nonwoven web is a web of meltblown fibers, it may include meltblown microfibers. The nonwoven web may be made of fiber forming polymers such as, for example, polyolefins. U.S. Pat. No. 5,916,661, entitled “Selectively Apertured Nonwoven Web” issued to Benson et al. on Jun. 29, 1999, discloses a process for selectively aperturing a nonwoven web and is incorporated herein by reference.
In another embodiment, the strip of material may be formed by a substance encapsulation system. U.S. Pat. No. 6,716,498, entitled “Applications For Substance Encapsulating Laminate Web” issued to Curro et al. on Apr. 6, 2004, disclosed a suitable substance application system and is incorporated herein by reference.
Surprisingly, we have found that strips of material with a SELF'd backing layer can be more easily stretched without causing sudden necking. Rather, the strip of material according to the present disclosure is uniformly deformed when it is stretched. These beneficial properties can be quantified by measuring certain characteristics of a strip of material, including Young's Modulus, % Strain@Break and % Strain@Yield. Strips of material according to the present disclosure may have a Young's Modulus of less than 50 MPa, in another embodiment less than 40 MPa, in yet another embodiment less than 30 MPa, and in yet another embodiment from about 15 MPa to about 50 MPa. In another embodiment, strips of material according to the present disclosure may have a % Strain@Break of greater than about 250%, in another embodiment of from about 250% to about 500% and in another embodiment of from about 200% to about 400%. In another embodiment, strips of material according to the present disclosure may have a % Strain@Yield of greater than about 25%, in another embodiment of from about 20% to about 300%, in another embodiment of from about 25% to about 200%, and in another embodiment of from about 30% to about 100%.
Oral Care Composition
The oral care composition is a composition, compound, or mixture capable of influencing or effecting a desired change in appearance and/or structure of the surface it contacts. Examples of appearance and structural changes include, but are not necessarily limited to, whitening, stain bleaching, stain removal, plaque removal, and tartar removal. According to the present disclosure, the oral care composition may be adhesive or non-adhesive and includes one or more oral care actives. In one embodiment, the active is for the whitening of the tooth surfaces.
Adhesive Composition
The adhesive is a composition, compound, or mixture capable of influencing or effecting a desired change in appearance and/or structure of the surface it contacts. Examples of appearance and structural changes include, but are not necessarily limited to, whitening, stain bleaching, stain removal, plaque removal, and tartar removal. According to the present disclosure, the adhesive composition includes one or more oral care actives. In one embodiment, the active is for the whitening of the tooth surfaces.
The adhesive composition may be coated on the strip of material, be applied by the user to the backing layer, or be applied by the user to their teeth and then the backing layer is placed over the coated teeth. The amount of adhesive applied to the backing layer or teeth will depend upon the size and capacity of the piece of material, concentration of the active, and the desired benefit. Generally, less than about 1 gram of substance is required. In certain embodiments, from about 0.05 grams to about 0.5 grams or from about 0.1 gram to about 0.4 grams of the substance is used. The amount of substance per square cm of material may be less than about 0.2 grams/cm2, from about 0.005 to about 0.1 grams/cm2, or from about 0.01 grams/cm2 to about 0.04 grams/cm2.
The adhesive may be in the form of a viscous liquid, paste, gel, aqueous gel, solution, or other suitable form that can provide sufficient adhesion. The substance may have a viscosity of from about 200 to about 1,000,000 cps, from about 100,000 to about 800,000 cps and more preferably from about 400,000 to about 600,000 cps at low shear rates (less than one 1/seconds).
In one embodiment, the adhesive composition may be an aqueous gelling agent. These gelling agents are safe for oral use, do not readily dissolve in saliva, and do not react with or inactivate the oral care compounds incorporated into them. Generally, the gelling agent is a swellable polymer. Furthermore, the gel formed with these agents provide sufficient adhesive attachment of the backing layer to the targeted area of the mouth. The level of gelling agent to form the gel composition is from about 0.1% to about 15%, in another embodiment from about 1% to about 10%, in another embodiment from about 2% to about 8%, and in yet another embodiment from about 4% to about 6%, by weight of the oral care composition or substance.
Suitable gelling agents include carboxypolymethylene, carboxymethyl cellulose, carboxypropyl cellulose, polyoxamers, carrageenan, Veegum, carboxyvinyl polymers, and natural gums such as gum karaya, xanthan gum, Guar gum, gum arabic, gum tragacanth, and mixtures thereof. In one embodiment, carboxypolymethylene obtained from B. F. Goodrich Company under the tradename Carbopol® is used. For example, Carbopols include Carbopol 934, 940, 941, 956 and mixtures thereof. Carboxypolymethylene is a slightly acidic vinyl polymer with active carboxyl groups. The normal concentration of various carboxypolymethylene resins in water, according to the manufacturer, is below about 2%. However, it has been found that by preparing supersaturated carboxypolymethylene compositions having an absolute concentration in the ranges specified above, suitable high viscosity oral gel compositions may be prepared.
The concentrated carboxypolymethylene gels have a number of important characteristics in addition to high viscosity. Enough carboxypolymethylene is added to the oral gel compositions beyond that required to provide high viscosity such that a significant quantity of saliva or water is required to lower the viscosity to the point that the composition may be diluted and washed out by saliva. The concentrated carboxypolymethylene composition also has a unique tackiness or stickiness which retains and seals the strip material against the targeted oral cavity surface it is affixed to, particularly teeth. However, care should be taken to avoid too much carboxypolymethylene thereby making insertion or withdrawal of the strip material difficult.
If the adhesive composition is an aqueous gel, the water present in the gel compositions should be deionized and free of organic impurities. Water comprises from about 0.1% to 95%, in another embodiment from about 5% to about 90%, and in yet to another embodiment from about 10% to about 80%, by weight of the oral care substance. This amount of water includes the free water that is added plus that amount that is introduced with other materials.
A pH adjusting agent may also be added to optimize the storage stability of the gel and to make the substance safe for oral tissue. These pH adjusting agents, or buffers, can be any material which is suitable to adjust the pH of the adhesive composition. Suitable materials include sodium bicarbonate, sodium phosphate, sodium hydroxide, ammonium hydroxide, sodium stannate, triethanolamine, citric acid, hydrochloric acid, sodium citrate, and combinations thereof. The pH adjusting agents are added in sufficient amounts so as to adjust the pH of the gel composition to about 4.5 to about 11, in another embodiment from about 5.5 to about 8.5, and in another embodiment from about 6 to about 7. pH adjusting agents are generally present in an amount of from about 0.01% to about 15% and in another embodiment from about 0.05% to about 5%, by weight of the adhesive composition.
While the gel described above provides sufficient adhesiveness, additional gelling agents may also be included in the formula to help the active ingredients adhere to the tissues of the oral cavity. Suitable agents include both polymers with limited water solubility as well as polymers lacking water solubility. These polymers deposit a thin film on both the oral cavity's soft and hard tissues when saliva combines with the instant composition. Suitable limited water solubility adhesives include: hydroxy ethyl or propyl cellulose. Adhesives lacking water solubility include: ethyl cellulose and polyox resins. Another possible adhesive suitable for use in the instant composition is polyvinylpyrrolidone with a molecular weight of about 50,000 to about 30,000,000. Still another possible adhesive suitable for use in the instant composition is a combination of Gantrez and the semisynthetic, water-soluble polymer carboxymethyl cellulose.
An additional carrier material may also be added to the adhesive composition, Carrier materials can be humectants. Suitable humectants include glycerin, sorbitol, polyethylene glycol, propylene glycol, and other edible polyhydric alcohols. Humectants are generally present in an amount of from about 10% to about 95% and in another embodiment from about 50% to about 80%, by weight of the adhesive composition. In addition to the above materials of the gel, a number of other components can also be added to the adhesive composition. Additional components include, but are not limited to, flavoring agents, sweetening agents, xylitol, opacifiers, coloring agents, and chelants such as ethylenediaminetetraacetic acid. These additional ingredients can also be used in place of the compounds disclosed above.
Oral Care Actives
As mentioned above, the oral care composition may include an oral care active at a level where upon directed use, promotes the benefit sought by the wearer without detriment to the oral surface it is applied to. Suitable for oral care actives include any material that is generally considered as safe for use in the oral cavity that provides changes to the overall health of the oral cavity, and specifically the condition of the oral surfaces the adhesive composition contacts. The level of oral care active is from about 0.01% to about 40%, in another embodiment from about 0.1% to about 30%, in another embodiment from about 0.5% to about 20%, and in yet another embodiment from about 1% to about 15%, by weight of the adhesive composition.
The following is a non all-inclusive list of oral care actives that may be used according to the present disclosure.
1. Teeth Whitening Actives
Teeth whitening actives may be included in the oral care substance. The actives suitable for whitening are selected from the group consisting of the peroxides, metal chlorites, perborates, percarbonates, peroxyacids, and combination thereof. Suitable peroxide compounds include hydrogen peroxide, calcium peroxide, carbamide peroxide, and mixtures thereof. Suitable metal chlorites include calcium chlorite, barium chlorite, magnesium chlorite, lithium chlorite, sodium chlorite, and potassium chlorite. Additional whitening actives may be hypochlorite and chlorine dioxide.
2. Phosphates
Anti-tartar agents known for use in dental care products includes phosphates. Phosphates include pyrophosphates, polyphosphates, polyphosphonates and mixtures thereof. Pyrophosphates are among the best known for use in dental care products. Pyrophosphate ions are delivered to the teeth derive from pyrophosphate salts. The pyrophosphate salts useful in the present compositions include the dialkali metal pyrophosphate salts, tetra-alkali metal pyrophosphate salts, and mixtures thereof. Disodium dihydrogen pyrophosphate (Na2H2P2O7), tetrasodium pyrophosphate (Na4P2O7), and tetrapotassium pyrophosphate (K4P2O7) in their unhydrated as well as hydrated forms are examples.
The pyrophosphate salts are described in more detail in Kirk & Othmer, Encyclopedia of Clinical Technology Third Edition, Volume 17, Wiley-Interscience. Publishers (1982), incorporated herein by reference in its entirety, including all references incorporated into Kirk & Othmer. Additional anticalculus agents include pyrophosphates or polyphosphates disclosed in U.S. Pat. No. 4,590,066 issued to Parran & Sakkab on May 20, 1986; polyacrylates and other polycarboxylates such as those disclosed in U.S. Pat. No. 3,429,963 issued to Shedlovsky on Feb. 25, 1969 and U.S. Pat. No. 4,304,766 issued to Chang on Dec. 8, 1981; and U.S. Pat. No. 4,661,341 issued to Benedict & Sunberg on Apr. 28, 1987; polyepoxysuccinates such as those disclosed in U.S. Pat. No. 4,846,650 issued to Benedict, Bush & Sunberg eon Jul. 11, 1989; ethylenediaminetetraacetic acid as disclosed in British Patent No. 490,384 dated Feb. 15, 1937; nitrilotriacetic acid and related compounds as disclosed in U.S. Pat. No. 3,678,154 issued to Widder & Briner on Jul. 18, 1972; polyphosphonates as disclosed in U.S. Pat. No. 3,737,533 issued to Francis on Jun. 5, 1973, U.S. Pat. No. 3,988,443 issued to Ploger, Schmidt-Dunker & Gloxhuber on Oct. 26, 1976 and U.S. Pat. No. 4,877,603 issued to Degenhardt & Kozikowski on Oct. 31, 1989; all of these patents are incorporated herein by reference. Anticalculus phosphates include potassium and sodium pyrophosphates; sodium tripolyphosphate; diphosphonates, such as ethane-1-hydroxy-1,1-diphosphonate, 1-azacycloheptane-1,1-diphosphonate, and linear alkyl diphosphonates; linear carboxylic acids; and sodium zinc citrate.
Agents to may be used in place of or in combination with the pyrophosphate salt include such known materials as synthetic anionic polymers including polyacrylates and copolymers of maleic anhydride or acid and methyl vinyl ether (e.g., Gantrez), as described, for example, in U.S. Pat. No. 4,627,977, to Gaffar et al., the disclosure of which is incorporated herein by reference in its entirety; as well as, e.g., polyamino propoane sulfonic acid (AMPS), zinc citrate trihydrate, polyphosphates (e.g., tripolyphosphate; hexametaphosphate), diphosphonates (e.g., EHDP; AHP), polypeptides (such as polyaspartic and polyglutamic acids), and mixtures thereof.
3. Fluoride Ion Source
Fluoride on sources are well known for use in oral care compositions as anti-caries agents. Fluoride ions are contained in a number of oral care compositions for this purpose, particularly toothpastes. Patents disclosing such toothpastes include U.S. Pat. No. 3,538,230, Nov. 3, 1970 to Pader et al; U.S. Pat. No. 3,689,637, Sep. 5, 1972 to Pader; U.S. Pat. No. 3,711,604, Jan. 16, 1973 to Colodney et al; U.S. Pat. No. 3,911,104, Oct. 7, 1975 to Harrison; U.S. Pat. No. 3,935,306, Jan. 27, 1976 to Roberts et al; and U.S. Pat. No. 4,040,858, Aug. 9, 1977 to Wason.
Application of fluoride ions to dental enamel serves to protect teeth against decay. A wide variety of fluoride ion-yielding materials can be employed as sources of soluble fluoride in the instant compositions. Examples of suitable fluoride ion-yielding materials are found in Briner et al; U.S. Pat. No. 3,535,421; issued Oct. 20, 1970 and Widder et al; U.S. Pat. No. 3,678,154; issued Jul. 18, 1972, both patents being incorporated herein by reference, in one embodiment, the instant compositions provide from about 50 ppm to 10,000 ppm, and in another embodiment from about 100 to 3000 ppm, of fluoride ions in the aqueous solutions that contact dental surfaces when used with the strip of material used in the mouth.
4. Antimicrobial Agents
Antimicrobial agents can also be included in oral care substances according to the present disclosure. Such agents may include, but are not limited to, 5-chloro-2-(2,4-dichlorophenoxy)-phenol, commonly referred to as triclosan, and described in The Merck Index, 11th ed. (1989), pp. 1529 (entry no. 9573) in U.S. Pat. No. 3,506,720, and in European Patent Application No. 0,251,591 of Beecham Group, PLC, published Jan. 7, 1988; phthalic acid and its salts including, but not limited to those disclosed in U.S. Pat. No. 4,994,262, Feb. 19, 1991, substituted monoperthalic acid and its salts and esters as disclosed in U.S. Pat. No. 4,990,329, Feb. 5, 1991, U.S. Pat. No. 5,110,583, May 5, 1992 and U.S. Pat. No. 4,716,035, Dec. 29, 1987, all to Sampathkumar; preferably magnesium monoperoxy phthalate, chlorhexidine (Merck Index, no. 2090), alexidine (Merck Index, no. 222; hexetidine (Merck Index, no. 4624); sanguinarine (Merck index, no. 8320); benzalkonium chloride (Merck Index, no. 1066); salicylanilide (Merck index, no. 8299); domiphen to bromide (Merck Index, no. 3411); cetylpyridinium chloride (CPC) (Merck Index, no. 2024; tetradecylpyridinium chloride (TPC); N-tetradecyl-4-ethylpyridinium chloride (TDEPC); octenidine; delmopinol, octapinol, and other piperidino derivatives; nicin preparations; zinc/stannous ion agents; antibiotics such as augmentin, amoxicillin, tetracycline, doxycycline, minocycline, and metronidazole; and analogs and salts of the above; essential oils including thymol, geraniol, carvacrol, citral, hinokitiol, eucalyptol, catechol (particularly 4-allyl catechol) and mixtures thereof; methyl salicylate; hydrogen peroxide; metal salts of chlorite and mixtures of all of the above.
5. Anti-Inflammatory Agents
Anti-inflammatory agents can also be present in the oral care substances. Such agents may include, but are not limited to, non-steroidal anti-inflammatory agents or NSAIDs such as ketorolac, flurbiprofen, ibuprofen, naproxen, indomethacin, aspirin, ketoprofen, piroxicam and meclofenamic acid. Use of NSAIDs such as Ketorolac are claimed in U.S. Pat. No. 5,626,838, issued May 6, 1997, herein incorporated by reference. Disclosed therein are methods of preventing and, or treating primary and reoccurring squamous cell carcinoma of the oral cavity or oropharynx by topical administration to the oral cavity or oropharynx an effective amount of an NSAID.
6. Nutrients
Nutrients may improve the condition of the oral cavity and can be included in the oral care substances. Nutrients include minerals, vitamins, oral nutritional supplements, enteral nutritional supplements, and mixtures thereof.
Minerals that can be included with the compositions of the present invention include calcium, phosphorus, fluoride, zinc, manganese, potassium and mixtures thereof. These minerals are disclosed in Drug Facts and Comparisons (loose leaf drug information service), Wolters Kluer Company, St. Louis, Mo., 1997, pp 10-17; incorporated herein by reference.
Vitamins can be included with minerals or used separately. Vitamins include Vitamins C and D, thiamine, riboflavin, calcium pantothenate, niacin, folic acid, nicotinamide, pyridoxine, cyanocobalamin, para-aminobenzoic acid, bioflavonoids, and mixtures thereof. Such vitamins are disclosed in Drug Facts and Comparisons (loose leaf to drug information service), Wolters Kluer Company, St. Louis, Mo., 1997, pp. 3-10; incorporated herein by reference.
Oral nutritional supplements include amino acids, lipotropics, fish oil, and mixtures thereof, as disclosed in Drug Facts and Comparisons (loose leaf drug information service), Wolters Kluer Company, St. Louis, Mo., 1997, pp. 54-54e; incorporated herein by reference. Amino acids include, but, are not limited to L-Tryptophan, L-Lysine, Methionine, Threonine, Levocarnitine or L-carnitine and mixtures thereof. Lipotropics include, but, are not limited to choline, inositol, betaine, linoleic acid, linolenic acid, and mixtures thereof. Fish oil contains large amounts of Omega-3 (N-3) Polyunsaturated fatty acids, eicosapentaenoic acid and docosahexaenoic acid.
Entenal nutritional supplements include, but, are not limited to protein products, glucose polymers, corn oil, safflower oil, medium chain triglycerides as disclosed in Drug Facts and Comparisons (loose leaf drug information service), Wolters Kluer Company, St. Louis, Mo., 1997, pp. 55-57; incorporated herein by reference.
7. Enzymes
An individual or combination of several compatible enzymes can be included in the oral care substances. Enzymes are biological catalysts of chemical reactions in living systems. Enzymes combine with the substrates on which they act forming an intermediate enzyme-substrate complex. This complex is then converted to a reaction product and a liberated enzyme which continues its specific enzymatic function.
Enzymes provide several benefits when used for cleansing of the oral cavity. Proteases break down salivary proteins which are absorbed onto the tooth surface and form the pellicle; the first layer of resulting plaque. Proteases along with lipases destroy bacteria by lysing proteins and lipids which form the structural component of bacterial cell walls and membranes. Dextranases break down the organic skeletal structure produced by bacteria that forms a matrix for bacterial adhesion. Proteases and amylases, not only present plaque formation, but also prevent the development of calculus by breaking-up the carbohydrate-protein complex that binds calcium, preventing mineralization.
Enzymes useful in the present disclosure include any of the commercially available proteases, glucanohydrolases, endoglycosidases, amylases, mutanases, lipases to and mucinases or compatible mixtures thereof. Preferred are the proteases, dextranases, endoglycosidases and mutanases, most preferred being papain, endoglycosidase or a mixture of dextranase and mutanase. Additional enzymes suitable for use in the present invention are disclosed in U.S. Pat. No. 5,000,939 to bring et al., Mar. 19, 1991; U.S. Pat. No. 4,992,420 to Neeser, Feb. 12, 1991; U.S. Pat. No. 4,355,022 to Rabussay, Oct. 19, 1982; U.S. Pat. No. 4,154,815 to Pader, May 15, 1979; U.S. Pat. No. 4,058,595 to Colodney, Nov. 15, 1977; U.S. Pat. No. 3,991,177 to Virda et al., Nov. 9, 1976 and U.S. Pat. No. 3,696,191 to Weeks, Oct. 3, 1972; all incorporated herein by reference.
8. Mouth and Throat Products
Other materials that can be used include commonly known mouth and throat products. Such products are disclosed in Drug Facts and Comparisons (loose leaf drug information service), Wolters bluer Company, St. Louis, Mo., 1997, pp. 520b-527; incorporated herein by reference. These products include, but, are not limited to anti-fungal, antibiotic and analgesic agents.
9. Antioxidants
Antioxidants are generally recognized as useful in oral care substances. Antioxidants are disclosed in texts such as Cadenas and Packer, The Handbook of Antioxidants©, 1996 by Marcel Dekker, Inc., incorporated herein by reference. Antioxidants that may be included in the oral care composition or substance of the present invention include, but are not limited to Vitamin E, ascorbic acid, Uric acid, carotenoids, Vitamin A, flavonoids and polyphenols, herbal antioxidants, melatonin, aminoindoles, lipoic acids and mixtures thereof.
10. H-2 Antagonists
Histamine-2 (H-2 or H2) receptor antagonist compounds (H-2 antagonists) may be used in the oral care composition of the present invention. As used herein, selective H-2 antagonists are compounds that block H-2 receptors, but do not have meaningful activity in blocking histamine-1 (H-1 or H1) receptors. Selective H-2 antagonists stimulates the contraction of smooth muscle from various organs, such as the gut and bronchi; this effect can be suppressed by low concentrations of mepyramine—a typical antihistaminic drug. The pharmacological receptors involved in these mepyramine-sensitive histamine to responses have been defined as H-1 receptors (Ash, A. S. F. & H. O, Schild, Brit. J. Pharmacol Chemother., Vol. 27 (1966), p. 427, incorporated herein by reference). Histamine also stimulates the secretion of acid by the stomach (Loew, E. R. &. O. Chickering, Proc. Soc. Exp. Biol. Med., Vol. 48 (1941), p. 65, incorporated herein by reference), increases the heart rate (Trendelenburg, U., J. Pharmacol., Vol. 130 (1960), p. 450, incorporated herein by reference), and inhibits contractions in the rat uterus (Dews, P. B. & J. D. P. Graham, Brit. J. Pharmacol. Chemother., Vol. 1 (1946), p. 278, incorporated herein by reference); these actions cannot be antagonized by mepyramine and related drugs. The H-2 antagonists useful in the oral care compositions or substances are those that blockade the receptors involved in mepyramine-insensitive, non-H-1 (H-2), histamine responses, and do not blockade the receptors involved in mepyramine-sensitive histamine responses.
Selective H-2 antagonists are those compounds found to be H-2 antagonists through their performance in classical preclinical screening tests for H-2 antagonist function. Selective H-2 antagonists are identified as compounds which can be demonstrated to function as competitive or non-competitive inhibitors of histamine-mediated effects in those screening models specifically dependent upon H-2 receptor function, but to lack significant histamine antagonist activity in those screening models dependent upon H-1 receptor function. Specifically, this includes compounds that would be classified as described by Black, J. W., W. A. M. Duncan, C. J. Durant, C. R. Ganellin & E. M. Parsons, “Definition and Antagonism of Histamine H-2-Receptors”, Nature, Vol. 236 (Apr. 21, 1972), pp. 385-390 (Black), incorporated herein by reference, as H-2 antagonists if assessed as described by Black through testing with the guinea pig spontaneously beating right atria in vitro assay and the rat gastric acid secretion in vivo assay, but shown to lack in significant H-1 antagonist activity relative to H-2 antagonist activity, if assessed as described by Black with either the guinea pig ileum contraction in vitro assay or the rat stomach muscle contraction in vivo assay. Preferably selective H-2 antagonists demonstrate no significant H-1 activity at reasonable dosage levels in the above H-1 assays. Typical reasonable dosage level is the lowest dosage level at which 90% inhibition of histamine, preferably 99% inhibition of histamine, is achieved in the above H-2 assays.
Selective H-2 antagonists include compounds meeting the above criteria which are to disclosed in U.S. Pat. Nos. 5,294,433 and 5,364,616 Singer et al., issued Mar. 15, 1994 and Nov. 15, 1994 respectively and assigned to Procter &. Gamble; both herein incorporated by reference, wherein the selective H-2 antagonist is selected from the group consisting of cimetidine, etintidine, ranitidine, ICIA-5165, tiotidine, ORE-17578, lupitidine, donetidine, famotidine, roxatidine, pifatidine, lamtidine, BL-6548 BMY-25271, zaltidine, nizatidine, mifentidine, BMY-52368, SKF-94482, BL-6341A, ICI-162846, ramixotidine, Wy-45727, SR-58042, BMY-25405, loxtidine, DA-4634, bisfentidine, sufotidine, ebrotidine, HE-30-256, D-16637, FRG-8813, FRG-8701, impromidine, L-643728, and FH-408.4. Particularly preferred is cimetidine (SKF-92334), N-cyano-N′-methyl-N″-(2-(((5-methyl-1H-imidazol-4-yl)methyl)thio)ethyl)guanidine:
##STR00001##
Cimetidine is also disclosed in the Merck Index, 11th edition (1989), p. 354 (entry no. 2279), and Physicians' Desk Reference, 46th edition (1992), p. 2228. Related preferred H-2 antagonists include burimamide and metiamide.
Release Liner
As mentioned above, the strip of material 810 may also include a release liner 827, as shown in
One suitable release liner is Scotchpak®, produced by 3M. The release liner may be cut to substantially the same size and shape as the backing layer or the release liner may be cut larger than the backing layer to provide a readily accessible means for separating the release liner from the backing layer. The release liner may be formed from a brittle material which cracks when the strip is flexed or from multiple pieces of material or a scored piece of material. Alternatively, the release liner may be in two overlapping pieces such as a typical adhesive strip bandage type design. A further description of materials suitable as release agents is found in Kirk-Othmer Encyclopedia of Chemical Technology, Fourth Edition, Volume 21, pp. 207-218, incorporated herein by reference.
The strip of material 810 may also include a flexible, fractured plastic film or mesh 816 located between the release liner and the backing layer, as shown in
The following examples are given solely for the purposes of illustration and are not to be construed as limitations of the present disclosure.
Examples 1-12 shown in Table 6 below are embodiments of oral care compositions for use with a strip in accordance with the present disclosure.
TABLE 6
Example Oral Care Compositions
1
2
3
4
5
6
Glycerin
10.000%
10.000%
20.000%
10.000%
—
—
Water
67.776%
64.348%
54.348%
64.248%
74.148%
67.776%
Hydrogen Peroxide (35%
15.143%
18.571%
18.571%
18.571%
18.571%
15.143%
Solution)
Carboxypolymethylene
4.500%
4.500%
4.500%
4.500%
4.500%
4.500%
Sodium Hydroxide (50%
2.000%
2.000%
2.000%
2.000%
2.000%
2.000%
Solution)
Sodium Saccharin
—
—
—
0.100%
0.200%
—
Sodium Stannate
0.200%
0.200%
0.200%
0.200%
0.200%
0.200%
Sodium Pyrophosphate
0.381%
0.381%
0.381%
0.381%
0.381%
0.381%
Propylene Glycol
—
—
—
—
—
10.000%
Pluronic 407
—
—
—
—
—
—
7
8
9
10
11
12
Glycerin
10.000%
—
3.000%
15.000%
10.000%
10.000%
Water
68.157%
57.276%
72.576%
63.076%
72.919%
66.955%
Hydrogen Peroxide (35%
15.143%
15.143%
17.143%
15.143%
—
17.143%
Solution)
Carboxypolymethylene
4.500%
—
4.500%
4.500%
4.500%
4.500%
Sodium Hydroxide (50%
2.000%
2.000%
2.200%
1.700%
2.000%
—
Solution)
Sodium Saccharin
—
—
—
—
—
—
Sodium Stannate
0.200%
0.200%
0.200%
0.200%
0.200%
—
Sodium Pyrophosphate
—
0.381%
0.381%
0.381%
0.381%
—
Propylene Glycol
—
—
—
—
—
—
Pluronic 407
—
25.000%
—
—
—
—
Potassium Hydroxide
—
—
—
—
—
1.403%
Carbamide Peroxide
—
—
—
—
10.000%
—
For Table 6 above, the values of peroxide active percentages and concentrations are measured using the following method. The package containing the peroxide system is stored for the stated period of time (e.g., 12 months) and conditions. After the stated storage time period, the peroxide concentration is measured using the Iodometric titration method. The Iodometric titration method is a standard method known in the art for measuring peroxide concentration. In general, the method is performed by weighing the substrate and composition containing the peroxide active, dissolving the composition in 1M sulfuric acid, and reacting the peroxide with an excess of potassium iodide in the presence of ammonium molybdate. This is then titrated with a known concentration of sodium thiosulfate to a clear endpoint using a starch indicator. The substrate is weighed upon completion of the titration and the composition weight is determined by difference. The peroxide concentration in the composition is then calculated. When the storage period is long, the concentration of the peroxide active can alternatively be determined by measuring the concentration as described above after at least one hundred and twenty days and then extrapolating for the remainder of the period using first order kinetics, as is known in the art. The above-described method is performed just after manufacture of a peroxide product and at the end of the specified storage period in order to determine the absolute peroxide concentrations as well as the percentage of the original concentration remaining, as is known in the art.
Examples 13-15 shown below are embodiments of oral care compositions for use with a strip in accordance with the present disclosure.
The following abbreviations and tradenames are used in the following examples:
Eudragit L 100-55 methacrylic acid copolymer, (Rohm America Inc.)
PEG polyethylene glycol 400
PVP30 Plasdone® K30 polyvinylpyrrolidone (ISP)
PVP90 Kollidon® 90F polyvinylpyrrolidone (BASF)
The following composition for tooth whitening was prepared from the following ingredients using a melt extrusion process:
*Eudragit L 100-55
9 wt %
PVP90
44 wt %
PEG
22 wt %
Hydrogen peroxide
6 wt %
Water, stabilizers, pH modulators
19 wt %
The ingredients were melt processed in a Brabender single screw extruder as follows: The Eudragit L 100-55 was added to the extruder first, followed by PVP90 and PEG, at a temperature of 100 to 150° C. The composition was extruded to a thickness of 0.35 mm between two polyethylene terephthalate release liners. Hydrogen peroxide solution was added to the extruded film.
A composition for tooth whitening was prepared from the following ingredients (Formula A):
Deionized water
35.0 wt %
Ethanol
35.0 wt %
Eudragit L 100-55
4.00 wt %
PEG
1.00 wt %
PVP90
7.00 wt %
Carbamide peroxide
18.0 wt %
Sodium citrate
0.13 wt %
The composition was mixed in a Cole-Parmer high-torque low-speed lab mixer supplied with Teflon coated impeller (2 inches in diameter) as follows. Deionized water was mixed with ethanol, followed by the addition of PEG. Sodium citrate was then added under vigorous stirring conditions. Eudragit L 100-55 powder was added slowly (within 2-5 min) under vigorous stirring (500-600 rpm). After about 5-10 min (it is not necessary to wait until all Eudragit is dissolved), PVP90 powder was slowly added (within 5 min) The high stirring rate was maintained over 5-10 min. Carbamide peroxide powder was added (within 1-2 min) and the mixture stirred to obtain a homogeneous solution (approximately 30 minutes at 800-900 rpm). The solution was then stored over a period of 2-5 hours to let the air bubbles dissipate.
A composition for tooth whitening was prepared from the following ingredients (Formula B):
Deionized water
35.0 wt %
Ethanol
35.0 wt %
Eudragit L 100-55
2.50 wt %
PEG
1.92 wt %
PVP90
6.00 wt %
Carbamide peroxide
18.0 wt %
Sodium Citrate
0.08 wt %
Methocel A4C
1.50 wt %
The composition was mixed in a Cole-Parmer high-torque low-speed lab mixer supplied with Teflon coated impeller (2 inches in diameter). Deionized water was mixed with ethanol, followed by the addition of PEG. Sodium citrate was then added under vigorous stirring conditions. Eudragit L 100-55 powder was added slowly (within 5 min) under vigorous stirring (500-600 rpm), followed by the slow (within 5 min) addition of Methocel A4C powder under vigorous stirring (500-600 rpm). After about 10 min, PVP90 powder was slowly added (within 5 min). The high stirring rate was maintained over 5-10 min. Carbamide peroxide powder was added (within 1-2 min) and the mixture stirred to obtain a homogeneous solution (approximately 30-60 minutes at 500-800 rpm). The solution was then stored over a period of 2-5 hours to let the air bubbles dissipate.
The following Examples (16-30) in Table 7 provide a comparison between teeth whitening strips that are commercially available to strips of material for the delivery of an oral care active according to the present disclosure.
TABLE 7
Young's
Thickness
Modulus
% Strain
% Strain
Example
mm
MPa
@Break %
@ Yield %
16
0.20
19
346
60
17
0.20
21
302
267
18
0.20
45
324
35
19
0.20
62
45
31
20
0.20
29
193
141
21
0.08
294
21
8
22
0.19
44
64
39
23
0.13
440
24
8
24
0.20
25
388
22
25
0.20
22
944
16
26
0.18
68
31
27
27
0.41
68
97
83
28
0.94
81
60
25
29
0.87
95
59
24
30
0.24
46
396
7
Examples 16-18 are embodiments of strips of material for the delivery of an oral care active in accordance with the present disclosure. These Examples were made using Example No. 12 in Table 3 as the backing layer. Example 17 was aged in a roll stock for an additional 3 weeks more than Example 16. Example 18 also included a DELNET located between the release liner and the backing layer as shown in
Example 19 is a commercially available whitening strip sold by The Procter and Gamble Company under the trademark CREST 3D WHITE WHITESTRIPS ADVANCED SEAL PROFESSIONAL EFFECT (Lot #1116BT3).
Example 20 is a commercially available whitening strip sold by The Procter and Gamble Company under the trademark CREST WHITESTRIPS 3D WHITE GENTLE ROUTINE (Lot #2206BT2).
Example 21 is a commercially available whitening strip sold by McNeil-PPC, Inc. under the trademark REMBRANDT STAIN DISSOLVING STRIPS (Lot #0192RD).
Example 22 is a commercially available whitening strip sold by LG Health and Beauty under the trademark CLAREN DENTAL WHITENING SOLUTION—NIGHT EFFECT (Lot #041027).
Example 23 is a commercially available whitening strip sold by Lornamead, Inc. under the trademark NATURAL WHITE dSolve (Lot #T4L039).
Example 24 is a commercially available whitening strip sold by Onuge Oral Care (Guangzhou) Limited under the trademark DENTAL WHITENING STRIPS.
Example 25 is a commercially available whitening strip sold by Xiamen YYX Trading Co., Ltd. under the trademark HEIDELBERG WHITESTRIPS (Lot #B 110909).
Example 26 is a commercially available whitening strip sold by Walgreen Co. under the trademark WALGREENS DENTAL STRIPS (Lot #058021).
Example 27 is a commercially available whitening strip sold by Target Brands, Inc. under the trademark UP & UP ADVANCED PLUS WHITENING STRIPS (Lot #012657 A1).
Example 28 is a commercially available whitening strip sold by Wal-Mart Stores Inc. under the trademark EQUATE DENTAL WHITENING STRIPS (Lot #021007B2).
Example 29 is a commercially available whitening strip sold by The Kroger Co. under the trademark KROGER WHITENING WRAPS (Lot #021621B1).
Example 30 is a commercially available whitening strip sold by CAO Group Inc. under the trademark SHEER WHITE (Lot #120207).
The method for generating the resistive force-elongation/strain data for Table 7 is ASTM standard test method D 882—Tensile Testing of Thin Plastic Sheeting, as described above, with the following modifications: Load Cell is 100 N; Gauge Length (grip separation) is 1.0 inch; Test Speed is 15.0 mm/sec; and Specimen Dimensions are 6.5 mm width×25.4 mm length.
The following Examples in Tables 8 and 9 provide data for various teeth whitening strips measured according to the Strip Removal Test described in detail below.
TABLE 8
Strip Removal Results for Sample Teeth Whitening
Products-Amount of Material Remaining After Peel Test
Material
collected
Material left on glass rods (avg)
(avg)
Gel
Backing
Gel + Backing
Examples
Test
length (mm)
% length
Length (mm)
% length
wt (g)
Example 19
Initial Peel
0
0
0
0
0
from Table 7
After 30 min
0
0
0
0
0
in water
After 1 hr in
0
0
0
0
0
water
Example 17
Initial Peel
0
0
0
0
0
from Table 7
After 30 min
0
0
0
0
0
in water
After 1 hr in
0
0
0
0
0
water
Example 30
Initial Peel
48
96
40
80
0.0905
from Table 7
After 30 min
48
96
29
58
0.066
in water
After 1 hr in
42
84
21
42
0.0418
water
% length is calculated by material weight/strip weight on glass rods/50 mm
TABLE 9
Strip Removal Results for Sample Teeth Whitening Products - Peel
Force
Peel Force (N) (avg)
After 30 min
Examples
Initial Peel
in water
After 1 hr in water
Example 19 from
0.2570
0.2391
0.1861
Table 7
Example 17 from
0.4509
0.3751
0.3547
Table 7
Example 30 from
1.9849
0.9825
0.9039
Table 7
Example 20 from
0.0052
Not able to measure
Not able to
Table 7
measure
Example 24 from
0.0024
Not able to measure
Not able to
Table 7
measure
Example 25 from
0.0077
Not able to measure
Not able to
Table 7
measure
Consumers generally prefer teeth whitening products to be easily and cleanly removed from their teeth. One way to compare ease of removal/clean removal for teeth whitening strips is to measure peel force and amount of material remaining after peel test. As shown in Tables 8 and 9, a Strip Removal Test was performed on representative teeth whitening products and the strip removal results were calculated.
In one embodiment, strips of material for deliver of an oral care active according to the present disclosure may have an initial peel force of greater than about 0.05 N. In another embodiment, strips of material for deliver of an oral care active may have an initial peel force of greater than about 0.10 N. In another embodiment, strips of material for deliver of an oral care active may have an initial peel force of greater than about 0.20 N. In yet another embodiment, strips of material for deliver of an oral care active may have an initial peel force of greater than about 0.30 N. In another embodiment, strips of material for deliver of an oral care active may have an initial peel force of greater than about 0.40 N. In another embodiment, strips of material for deliver of an oral care active may have an initial peel force of from about 0.05 N to about 1.0 N and in another embodiment from about 0.10 N to about 0.60N.
In one embodiment, strips of material for deliver of an oral care active according to the present disclosure may have less than about 0.05 g of material (gel+backing layer) remaining after an initial peel test. In another embodiment, strips of material for deliver of an oral care active may have less than about 0.025 g of material remaining after an initial peel test. In another embodiment, strips of material for deliver of an oral care active may have about 0.0 g of material remaining after an initial peel test. In another embodiment, strips of material for deliver of an oral care active may have from about 0.0 g to about 0.05 g of material remaining after an initial peel test.
Test Methods
The test methods and apparatus described below may be useful in testing embodiments of the present disclosure:
Two Cycle Hysteresis Test
This method is used to determine properties of strips of material, which may correlate with the forces experienced by the consumer during application and use. The two cycle hysteresis test is performed at room temperature (about 22° C.). The sample to be tested is cut into a substantially rectilinear shape, for example (approximately 0.20 mm thick, approximately 15 mm wide by approximately 76 mm long). A suitable instrument for this test includes a tensile tester from MTS Systems Corp., Eden Prairie, Minn., for example, Model Synergie 400. The instrument is interfaced with a computer. TestWorks 4™ software controls the testing parameters, performs data acquisition and calculations, and provides graphs and data reports.
The grips used for the test are wider than the sample. The grips are air actuated grips designed to concentrate the entire gripping force along a single line perpendicular to the direction of testing stress having one flat surface and an opposing face from which protrudes a half round (radius=6 mm) to minimize slippage of the sample.
The load cell is selected so that the forces measured will be between 10% and 90% of the capacity of the load cell or the load range used. A 100 Newton load cell may be used. The fixtures and grips are installed. The instrument is calibrated according to the manufacturer's instructions. The distance between the lines of gripping force (gauge length) is 2 inches (50.8 mm), which is measured with a steel ruler held beside the grips, unless specified otherwise. The load reading on the instrument is zeroed to account for the mass of the fixture and grips. The mass, thickness, and basis weight of the specimen are measured before testing. The specimen is mounted into the grips in a manner such that there is no slack and the load measured is between 0.00 Newton and 0.02 Newton, unless specified otherwise.
The two cycle hysteresis test method for strip samples involves the following steps (all strains are engineering strains):
(1) Strain the sample to 50% at a constant crosshead speed of 5 mm per second;
(2) Hold for 2 minutes;
(3) Reduce strain to 40% strain;
(4) Hold for 10 minutes.
A graph of two cycles is generated.
As can be seen from
Strip Removal Test
The Strip Removal Test is described as follows:
Equipment
The dimensions and values disclosed herein are not to be understood as being strictly limited to the exact numerical values recited. Instead, unless otherwise specified, each such dimension is intended to mean both the recited value and a functionally equivalent range surrounding that value. For example, a dimension disclosed as “40 mm” is intended to mean “about 40 mm”.
Every document cited herein, including any cross referenced or related patent or application, is hereby incorporated herein by reference in its entirety unless expressly excluded or otherwise limited. The citation of any document is not an admission that it is prior art with respect to any invention disclosed or claimed herein or that it alone, or in any combination with any other reference or references, teaches, suggests or discloses any such invention. Further, to the extent that any meaning or definition of a term in this document conflicts with any meaning or definition of the same term in a document incorporated by reference, the meaning or definition assigned to that term in this document shall govern.
While particular embodiments of the present invention have been illustrated and described, it would be obvious to those skilled in the art that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Zhao, Jean Jianqun, Sagel, Paul Albert, Nguyen, Lan Ngoc
| Patent | Priority | Assignee | Title |
| Patent | Priority | Assignee | Title |
| 1979119, | |||
| 2560724, | |||
| 2835628, | |||
| 2994362, | |||
| 3047966, | |||
| 3070102, | |||
| 3096202, | |||
| 3256014, | |||
| 3444858, | |||
| 3598123, | |||
| 3625215, | |||
| 3640741, | |||
| 3657413, | |||
| 3659928, | |||
| 3688406, | |||
| 3711182, | |||
| 3729839, | |||
| 3754332, | |||
| 3784390, | |||
| 3844286, | |||
| 3859987, | |||
| 3902509, | |||
| 3955281, | Dec 05 1974 | GILLETTE COMPANY THE, A CORP OF DE | Disposable dental tray for topical application of fluoride gel and other dental medications |
| 3964164, | Feb 05 1973 | Method of applying preventive and therapeutic agents | |
| 3972995, | Apr 14 1975 | American Home Products Corporation | Dosage form |
| 3998215, | Dec 18 1968 | Minnesota Mining and Manufacturing Company | Bio-medical electrode conductive gel pads |
| 4029757, | Dec 15 1975 | Hoffmann-La Roche Inc. | Manufacture of pharmaceutical unit dosage forms |
| 4029758, | Dec 15 1975 | Hoffmann-La Roche Inc. | Preparation of pharmaceutical unit dosage forms |
| 4031200, | Dec 15 1975 | Hoffmann-La Roche Inc. | Manufacture of pharmaceutical unit dosage forms |
| 4032627, | Apr 02 1973 | COSMOLAB, INC , 1100 GARRETT ROAD, LEWISBURG, TENNESSEE, 37091, A CORP OF TENNESSEE | Tooth whitening cosmetic composition |
| 4072551, | Dec 15 1975 | Hoffman-La Roche Inc. | Novel dosage form |
| 4084700, | Feb 06 1976 | Optarac Corporation | Display rack |
| 4136145, | Jul 05 1974 | Schering Aktiengesellschaft | Medicament carriers in the form of film having active substance incorporated therein |
| 4136162, | Jul 05 1974 | Schering Aktiengesellschaft | Medicament carriers in the form of film having active substance incorporated therein |
| 4138314, | Apr 10 1975 | BASF Corporation | Method of forming diaphragms from discrete thermoplastic fibers requiring no bonding or cementing |
| 4138814, | Dec 05 1974 | GILLETTE COMPANY THE, A CORP OF DE | Disposable dental tray for topical application of fluoride gel and other dental medications |
| 4139627, | Oct 06 1977 | BEECHAM INC A CORP OF | Anesthetic lozenges |
| 4182222, | Feb 16 1978 | Coupon confining bag method | |
| 4211330, | Feb 01 1979 | Oral health and hygiene kit | |
| 4232334, | May 22 1979 | Revlon Consumer Products Corporation | Cosmetic apparatus and method |
| 4251400, | Nov 03 1971 | ELMER S PRODUCTS, INC | Hot and cold water redispersible polyvinyl acetate adhesives |
| 4273418, | Nov 30 1979 | Mattel, Inc | Mirror for producing optical illusions |
| 4292299, | Nov 06 1978 | Teijin Limited | Slow-releasing medical preparation to be administered by adhering to a wet mucous surface |
| 4294820, | Jan 11 1979 | KEY PHARMACEUTICALS, INC | Polymeric diffusion matrix containing phenylephrine |
| 4307075, | Sep 13 1979 | American Home Products Corporation | Topical treatment of aphthous stomatitis |
| 4308250, | Nov 07 1978 | PFIZER, INC , A CORP OF NY | Sustained drug release device |
| 4324547, | Sep 16 1978 | Vishay Intertechnology, Inc. | Dentistry technique |
| 4325855, | Sep 10 1975 | Lingner and Fischer GmbH | Adhesives |
| 4331576, | Jan 29 1981 | SWIFT ADHESIVES, INC A DE CORPORATION | Water-soluble, pressure-sensitive, hot-melt adhesives |
| 4335731, | Jul 25 1978 | Device for oral hygiene care | |
| 4363843, | Mar 20 1979 | Raychem Limited | Seals |
| 4373036, | Dec 21 1981 | Block Drug Company, Inc. | Denture fixative composition |
| 4376628, | May 09 1979 | B.V. Gaba | Device for treating teeth |
| 4428373, | Feb 03 1982 | Sultan Dental Products Limited | Disposable dental tray |
| 4431631, | Jan 03 1983 | Colgate-Palmolive Company | Aqueous oral solution |
| 4438258, | Jun 12 1981 | British Technology Group Limited | Hydrogels |
| 4442258, | Jul 04 1979 | Nitto Electric Industrial Co., Ltd. | Water-soluble pressure-sensitive adhesive composition |
| 4460562, | Jan 11 1979 | Key Pharmaceuticals, Inc. | Polymeric diffusion matrix containing propranolol |
| 4482535, | Oct 03 1980 | Cosmetic preparation for teeth | |
| 4491479, | Nov 12 1982 | ADNOVUM AG, A SWISS COMPANY | Shaped semi-solid articles |
| 4503070, | Jul 31 1981 | Method for reducing the duration of the common cold | |
| 4515162, | Mar 14 1980 | Nitto Electric Industrial Co., Ltd. | Electrode pad |
| 4517173, | Sep 26 1980 | Nippon Soda Co. Ltd. | Mucous membrane-adhering film preparation and process for its preparation |
| 4518721, | Mar 26 1982 | Richardson-Vicks Inc. | Hydrophilic denture adhesive |
| 4522593, | Jul 07 1983 | ULTRADENT PRODUCTS, INC , 1345 EAST 3900 SOUTH, SALT LAKE CITY, UTAH 84124, A CORP OF UTAH | Knitted gingival retraction cord |
| 4522805, | Jun 08 1983 | Tooth and gum dentifrice | |
| 4522806, | Oct 10 1980 | CPPD, INC , A CORP OF IL | Oral compositions for hexetidine and zinc salts for the synergistic inhibition of dental plaque |
| 4528180, | Mar 01 1983 | BLOCK DRUG COMPANY, INC | Dental preparation, article and method for storage and delivery thereof |
| 4532063, | Aug 15 1983 | S. C. Johnson & Son, Inc. | Dissolvable bleach sheet |
| 4537778, | Jan 03 1983 | COLGATE-PALMOLIVE COMPANY, A CORP OF DE | Oral preparation |
| 4544354, | Sep 21 1984 | Anteriorly bridged dental trays | |
| 4554154, | Mar 15 1983 | Dental product and method of dental treatment | |
| 4557692, | Feb 12 1981 | Occlusal splints and the method of manufacturing the same | |
| 4560351, | Jul 05 1984 | Method of and apparatus for applying dental treatment fluid | |
| 4568536, | Feb 08 1985 | Ethicon, Inc. | Controlled release of pharmacologically active agents from an absorbable biologically compatible putty-like composition |
| 4592487, | Jul 03 1985 | WITKIN, ROY T ; SIMON, GILBERT I | Dentifrices |
| 4592488, | May 24 1985 | WITKIN, ROY T ; SIMON, GILBERT I | Method for the preparation of chemotherapeutic compositions for the treatment of periodontal disease, compositions therefor and use thereof |
| 4592726, | Jan 03 1983 | BRILLIANT ENTERPRISES, L L C | Diagnostic mirror and light filter |
| 4593053, | Dec 07 1984 | Medtronic, Inc. | Hydrophilic pressure sensitive biomedical adhesive composition |
| 4623394, | Apr 14 1984 | Kabushiki Kaisha Hayashibara Seibutsu Kagaku Kenkyujo | Gradually disintegrable molded article |
| 4640685, | Apr 15 1985 | Hand-held light filter | |
| 4650665, | Feb 08 1985 | Ethicon, Inc. | Controlled release of pharmacologically active agents from an absorbable biologically compatible putty-like composition |
| 4661070, | Mar 17 1986 | Demetron Research Corporation | Method for bleaching discolored teeth |
| 4687663, | Mar 01 1983 | CHURCH & DWIGHT CO , INC | Dental preparation, article and method for storage and delivery thereof |
| 4690996, | Aug 28 1985 | National Starch and Chemical Corporation | Inverse emulsions |
| 4696757, | Jun 16 1986 | American Home Products Corporation | Stable hydrogen peroxide gels |
| 4712460, | Nov 18 1985 | Roche Diagnostics Operations, Inc | Integrated drug dosage form and metering system |
| 4713239, | May 29 1979 | VSESOJUZNY KARDIOLOGICHESKY NAUCHNY TSENTR AKADEMII MEDITSINSKIKH NAUK SSSR; VSESOJUZNY NAUCHO-ISSLEDOVATELSKY I ISPYTATELNY INSTITUT MEDITSINSKOI TEKHNIKI | Antianginal film and method of treating ischemic heart disease |
| 4713243, | Jun 16 1986 | JOHNSON & JOHNSON CONSUMER PRODUCTS, INC | Bioadhesive extruded film for intra-oral drug delivery and process |
| 4722761, | Mar 28 1986 | NDM, INC | Method of making a medical electrode |
| 4728291, | Jun 26 1986 | Cloth wrap dental process | |
| 4741700, | Jul 16 1986 | Dental breath freshening device | |
| 4741941, | Nov 04 1985 | Kimberly-Clark Worldwide, Inc | Nonwoven web with projections |
| 4755385, | Jul 10 1985 | DR KARL THOMAE GMBH | Oral pharmaceutical preparations containing 9-deoxo-11-deoxy-9,11-[imino[2-(2-methoxyethoxy)-ethylidene]-oxy]-(9S)-e rythromycin |
| 4755386, | Jan 22 1986 | Schering Corporation | Buccal formulation |
| 4765983, | Jun 05 1985 | Astellas Pharma INC | Adhesive medical tapes for oral mucosa |
| 4770634, | Jun 11 1986 | LACLEDE, INC | Method for treating teeth with foamable fluoride compositions |
| 4772470, | Apr 27 1985 | Nitto Electric Industrial Co., Ltd.; Sunstar Inc. | Oral bandage and oral preparations |
| 4777046, | Oct 04 1984 | Nippon Kayaku Kabushiki Kaisha; Teikoku Seiyaku Kabushiki Kaisha; Kaken Pharmaceutical Co., Ltd. | Sheet-like preparation |
| 4786253, | Mar 09 1987 | HENNERET PROPERTIES PROPRIETARY LIMITED, 55 DE VILLIERS ST , VEREENIGING, TRANSVAAL PROVINCE, REP OF SOUTH AFRICA A CORP OF THE REP OF SOUTH AFRICA | Dental model articulator |
| 4788052, | Apr 17 1987 | Colgate-Palmolive Company | Stable hydrogen peroxide dental gel containing fumed silicas |
| 4799888, | Jun 26 1986 | Dental process with treated fabric | |
| 4812308, | Feb 20 1987 | Church & Dwight Co., Inc. | Hydrogen peroxide-releasing tooth powder |
| 4828113, | May 18 1988 | Dental treatment kit | |
| 4837008, | Sep 14 1983 | Peroxydent Group | Periodontal composition and method |
| 4839156, | Apr 17 1987 | Colgate-Palmolive Company | Stable hydrogen peroxide dental gel |
| 4839157, | Apr 17 1988 | Colgate-Palmolive Company | Stable hydrogen peroxide dental gel containing fumed silicas |
| 4849213, | Mar 01 1983 | BLOCK DRUG COMPANY, INC | Dental preparation, article and method for storage and delivery therof |
| 4849246, | Oct 09 1985 | LTS Lohmann Theraple-Systeme AG; LTS Lohmann Therapie-Systeme AG | Process for producing an administration or dosage form for drugs, reagents or other active ingredients |
| 4851394, | Dec 29 1986 | UNI FOOD SYSTEMS, INC | Glucomannan/polyhydric alcohol composition and film prepared therefrom |
| 4860754, | Apr 01 1987 | E. R. Squibb & Sons, Inc. | Electrically conductive adhesive materials |
| 4876092, | Feb 01 1986 | Teikoku Seiyaku Kabushiki Kaisha | Sheet-shaped adhesive preparation applicable to oral cavity |
| 4895517, | Apr 14 1987 | ULTRADENT PRODUCTS, INC , A CORP OF UTAH | Methods for performing vital dental pulpotomy |
| 4895721, | Jan 22 1988 | CHURCH & DWIGHT CO , INC | Peroxide gel dentifrice compositions |
| 4900253, | Jul 15 1987 | Dental mirror having ultraviolet filter | |
| 4900552, | Mar 30 1988 | WATSON LABORATORIES, INC , A NEVADA CORP | Mucoadhesive buccal dosage forms |
| 4900554, | Dec 24 1986 | TEIKOKU SEIYAKU CO , LTD , A CORP OF JAPAN | Adhesive device for application to body tissue |
| 4902227, | May 04 1988 | Pascal Company, Inc. | Dental treatment tray |
| 4910247, | Mar 27 1989 | ISP CAPITAL, INC | Adhesive composition |
| 4915950, | Feb 12 1988 | Ortho-McNeil Pharmaceutical, Inc | Printed transdermal drug delivery device |
| 4919615, | Apr 28 1989 | Orthodontic band cap | |
| 4925670, | Sep 09 1986 | LTS Lohmann Theraple-Systeme AG; LTS Lohmann Therapie-Systeme AG | Administration and dosage form for drug active agents, reagents or the like and process for the preparation thereof |
| 4927634, | Dec 16 1987 | Richardson-Vicks Inc. | Pharmaceutical compositions containing dyclonine HC1 and phenol |
| 4927636, | Nov 11 1986 | 501 Kabushiki Kaisha Hayashibara Kagaku Kenkyujo | Association complex comprising pullulan and polyethylene glycol, and preparation and uses of the same |
| 4931282, | Nov 25 1987 | Minnesota Mining and Manufacturing Company; MINNESOTA MINING AND MANUFACTURING COMPANY, SAINT PAUL, MINNESOTA, A CORP OF DE | Pressure-sensitive medical sealant |
| 4948580, | Dec 08 1988 | E. R. Squibb & Sons, Inc. | Muco-bioadhesive composition |
| 4968251, | Jul 03 1989 | 3M Innovative Properties Company | Treatment of a tooth |
| 4971782, | Sep 14 1983 | Peroxydent Group | Periodontal composition and method |
| 4972946, | Jan 08 1990 | Disposable dental hygiene kit | |
| 4978531, | Aug 13 1987 | WALTON S A , A CORP OF SPAIN | Clebopride transdermal patch |
| 4980152, | Aug 06 1987 | Marion Laboratories | Oral preparation |
| 4983379, | Mar 01 1983 | BLOCK DRUG COMPANY, INC | Dental preparation, article and method for storage and delivery thereof |
| 4983381, | Apr 16 1987 | FUTURA MEDICAL S A | Method and device for producing the whitening of live teeth with pathological and normal colorations |
| 4988500, | Sep 29 1989 | The Procter & Gamble Company; Procter & Gamble Company, The | Oral compositions |
| 4990089, | Aug 23 1988 | Dunhall Pharmaceuticals, Inc. | Method and material for brightening teeth |
| 5001170, | Dec 01 1989 | Warner-Lambert Company | Denture stabilizer |
| 5004631, | Jan 22 1986 | DSM IP ASSETS B V | Surface treatment with sulfonate ester polymer |
| 5024701, | Aug 08 1983 | Hercules Incorporated | Denture adhesive composition |
| 5047244, | Jun 03 1988 | Watson Laboratories, Inc. | Mucoadhesive carrier for delivery of therapeutical agent |
| 5059120, | Dec 19 1989 | Dental impression pads and method of manufacture | |
| 5059417, | Jun 26 1990 | CHURCH & DWIGHT CO , INC | Peroxide gel dentifrice |
| 5064717, | Apr 28 1989 | NEW OJI PAPER CO , LTD | Adhesive sheet |
| 5076791, | Oct 22 1990 | Professional home method for bleaching teeth | |
| 5084268, | Jun 17 1991 | Dental Concepts LLC | Tooth whitening dentifrice |
| 5098303, | Mar 22 1990 | Ultradent Products, Inc.; ULTRADENT PRODUCTS, INC , A CORP OF UT | Method for bleaching teeth |
| 5122365, | Feb 15 1989 | Natural White, Inc. | Teeth whitener |
| 5126066, | Jun 22 1988 | Akzo N.V. | Stable, pourable aqueous bleaching compositions comprising solid organic peroxy acids and at least two polymers |
| 5137729, | Jan 31 1989 | Nitto Denko Corporation | Drug preparation applicable to oral mucosa |
| 5158825, | Jul 13 1989 | Adherent insert for artificial teeth and process of manufacturing the insert | |
| 5160737, | May 03 1988 | DEXCEL PHARMA TECHNOLOGIES LTD ; Yissum Research Development Company of the Hebrew University of Jerusalem | Liquid polymer composition, and method of use |
| 5165424, | Aug 09 1990 | PERFECT SMILE CORPORATION | Method and system for whitening teeth |
| 5166233, | Jan 31 1989 | Nitto Denko Corporation; Sunstar K.K. | Film applicable to oral mucosa and drug preparation comprising the same |
| 5171564, | Sep 13 1991 | Colgate Palmolive Company | Aqueous tooth whitening dentifrice |
| 5186938, | Jul 24 1984 | Key Pharmaceuticals, Inc. | Adhesive transdermal dosage layer |
| 5192802, | Sep 25 1991 | McNeil-PPC, Inc. | Bioadhesive pharmaceutical carrier |
| 5211559, | Jul 18 1991 | Gillette Canada Company | Dental treatment tray for holding medicament gel |
| 5229164, | Dec 19 1985 | Capsoid Pharma GmbH | Process for producing individually dosed administration forms |
| 5234342, | Mar 22 1990 | Ultradent Products, Inc. | Sustained release method for treating teeth surfaces |
| 5246371, | Aug 31 1992 | Ultradent Products, Inc.; ULTRADENT PRODUCTS, INC , A CORP OF UT | Method and apparatus for delivery of highly filled, thixotropic sealant to teeth |
| 5252334, | Sep 08 1989 | Ortho-McNeil Pharmaceutical, Inc | Solid matrix system for transdermal drug delivery |
| 5256402, | Sep 13 1991 | Colgate-Palmolive Company | Abrasive tooth whitening dentifrice of improved stability |
| 5271940, | Sep 14 1989 | Ortho-McNeil Pharmaceutical, Inc | Transdermal delivery device having delayed onset |
| 5288231, | Mar 08 1993 | PINNACLE PRODUCTS, INC | Light shield for dental apparatus |
| 5288498, | May 01 1985 | UNIVERSITY OF UTAH RESEARCH FOUNDATION, A CORP OF UT | Compositions of oral nondissolvable matrixes for transmucosal administration of medicaments |
| 5290566, | Dec 18 1990 | LUSTERDENT, LLC | Tooth whitening formulation and method |
| 5302375, | Nov 19 1992 | Colgate-Palmolive Company; Colgate-Palmolive Co | Oral composition having improved tooth whitening effect |
| 5310563, | Oct 25 1991 | Colgate-Palmolive Company | Dental material and method for applying preventative and therapeutic agents |
| 5314915, | Sep 25 1991 | McNeil-PPC, Inc. | Bioadhesive pharmaceutical carrier |
| 5320831, | Dec 30 1992 | Procter & Gamble Company, The | Oral compositions |
| 5324342, | Apr 18 1989 | Daidotokushuko Kabushikikaisha | Method of refining molten chrome steel |
| 5326685, | Feb 13 1991 | SHOWA WATSUMEI KAISHA, LTD | Viscous fluid dispensing apparatus |
| 5330746, | May 03 1988 | DEXCEL PHARMA TECHNOLOGIES LTD ; Yissum Research Development Company of the Hebrew University of Jerusalem | Dental varnish composition, and method of use |
| 5332576, | Feb 27 1991 | Noven Pharmaceuticals, Inc. | Compositions and methods for topical administration of pharmaceutically active agents |
| 5340314, | Nov 27 1992 | Method of bonding and relining dentures | |
| 5340581, | Aug 23 1991 | GILLETTE COMPANY, THE | Sustained-release matrices for dental application |
| 5344702, | Sep 14 1990 | Hoechst Celanese Corp. | Coated fibers |
| 5345551, | Nov 09 1992 | i2z Technology, LLC | Method and system for synchronization of simultaneous displays of related data sources |
| 5356291, | Jul 03 1989 | 3M Innovative Properties Company | Treatment of a tooth |
| 5364267, | Feb 16 1993 | Ultradent Products, Inc.; Ultradent Products, INC | Syringe system for matching tooth composite colors |
| 5376006, | Mar 22 1990 | Ultradent Products, Inc. | Dental bleaching compositions and methods for bleaching teeth surfaces |
| 5380198, | Aug 06 1990 | Matrix for dental medicine and a device for the fabricaton of matrix bands | |
| 5387103, | Feb 16 1993 | Ultradent Products, Inc.; Ultradent Products, INC | Syringe apparatus for delivering tooth composites and other solid yet pliable materials |
| 5393528, | May 07 1992 | Dissolvable device for contraception or delivery of medication | |
| 5401495, | Oct 10 1990 | LORNAMEAD BRANDS, INC | Teeth whitener |
| 5401528, | Mar 19 1991 | Thera Patent GmbH & Co. KG Geselleschaft fur industrielle Schutzrechte | Use of compositions based on organically modified silicic acid polycondensates for coating teeth and dental prostheses |
| 5409631, | Mar 22 1990 | Ultradent Products | Dental bleaching compositions and methods for bleaching teeth surfaces |
| 5425641, | Jul 27 1993 | Ultradent Products, Inc. | Dental kit and process for sealing pits and fissures in enamel |
| 5425953, | Apr 23 1991 | DEXCEL PHARMA TECHNOLOGIES LTD | Polymer composition for tooth bleaching and other dental uses thereof |
| 5427770, | Nov 28 1988 | Chesebrough-Ponds USA Co., Division of Conopco, Inc. | Dentifrices containing amino alkyl silicones |
| 5433952, | May 04 1992 | Digestive Care Inc. | Intraoral medicament-releasing device |
| 5438076, | May 03 1988 | Yissum Research Development Company of the Hebrew University of Jerusalem | Liquid polymer composition, and method of use |
| 5455043, | Jun 13 1990 | Device for controlled release of vaporous medications through nasal route | |
| 5458879, | Mar 03 1994 | Procter & Gamble Company, The | Oral vehicle compositions |
| 5462749, | Sep 25 1991 | McNell-PPC, Inc. | Bioadhesive pharmaceutical carrier |
| 5464348, | Feb 16 1993 | Ultradent Products, Inc. | Syringe system for matching tooth composite colors |
| 5472704, | May 30 1991 | Recordati S.A., Chemical and Pharmaceutical Company | Pharmaceutical controlled-release composition with bioadhesive properties |
| 5474780, | Apr 27 1990 | Allergan | Monolithic maleic anhydride drug delivery systems |
| 5505933, | Jun 27 1994 | Colgate Palmolive Company | Desensitizing anti-tartar dentifrice |
| 5509800, | Aug 20 1993 | INVERTEC PTY LTD | Light-filter for dental use |
| 5522726, | Oct 27 1994 | Method for anesthetizing teeth | |
| 5529782, | May 07 1992 | Dissolvable device for contraception or delivery of medication | |
| 5534562, | Apr 07 1995 | Ultradent Products, Inc. | Compositions and methods for priming and sealing dental and biological substrates |
| 5560379, | Aug 12 1994 | Dental paper pick and flosser | |
| 5565190, | Nov 14 1994 | J A WOOLLAM CO , INC | Dentifrice compositions containing reactive ingredients stabilized with alkali metal compounds |
| 5575654, | Nov 24 1992 | OROSCIENCE, INC | Apparatus and method for lightening teeth |
| 5575655, | Jul 03 1989 | 3M Innovative Properties Company | Treatment of a tooth |
| 5579523, | Oct 13 1992 | Sony Corporation | Method for controlled locking/unlocking of a system using a locking mode flag during an interrupt routine |
| 5593684, | Aug 04 1993 | McNeil AB | Method and therapeutic system for smoking cessation |
| 5599552, | Jul 24 1989 | Atrix Laboratories, Inc. | Biodegradable polymer composition |
| 5599553, | Sep 01 1992 | Dong Kook Pharmaceutical Co., Ltd. | Local drug delivery film for periodontal treatment |
| 5603701, | Mar 27 1995 | Ultradent Products, Inc. | Syringe apparatus with threaded plunger for delivering tooth composites and other solid yet pliable materials |
| 5611687, | Nov 06 1995 | MEDTECH PRODUCTS, INC | Oral hygiene delivery system |
| 5614174, | Nov 14 1994 | Colgate Palmolive Company | Stabilized dentifrice compositions containing reactive ingredients |
| 5616027, | Apr 18 1995 | ARCHTEK DENTAL, LLC | Custom dental tray |
| 5618273, | Mar 27 1995 | Ultradent Product, Inc. | Syringe apparatus with threaded plunger for delivering tooth composites and other solid yet pliable materials |
| 5620322, | Jul 27 1995 | STEMMED IMPLANT TECHNOLOGY INC | Dental matrix strip |
| 5626866, | Mar 07 1994 | TheraTech, Inc. | Drug-containing adhesive composite transdermal delivery device |
| 5629003, | Jun 07 1990 | LTS Lohmann Therapie-Systeme AG | Rapidly disintegrating sheet-like presentations of multiple dosage units |
| 5631000, | Mar 11 1996 | LACLEDE PROFESSIONAL PRODUCTS, INC | Anhydrous tooth whitening gel |
| 5631055, | Oct 10 1990 | Minnesota Mining and Manufacturing Company | Paint masking assembly and method of masking |
| 5635162, | Feb 23 1995 | Ultradent Products, Inc. | Hemostatic composition for treating gingival area |
| 5639445, | Oct 25 1991 | Colgate-Palmolive Company | Dental material and method for applying preventative and therapeutic agents |
| 5648064, | Jul 07 1995 | Colgate-Palmolive Company | Oral compositions having accelerated tooth whitening effect |
| 5660178, | Dec 01 1992 | Minnesota Mining and Manufacturing Company | Hydrophilic pressure sensitive adhesives |
| 5662758, | Jan 10 1996 | The Procter & Gamble Company; Procter & Gamble Company, The | Composite material releasably sealable to a target surface when pressed thereagainst and method of making |
| 5678273, | Mar 20 1996 | DENTAL DOTS, INC | Disposable oral hygiene applicator |
| 5683680, | Nov 14 1994 | Colgate Palmolive Company | Dentifrice compositions containing reactive ingredients stabilized with alkali metal compounds |
| 5685712, | Jun 07 1995 | Ultradent Products, Inc. | Patient dentist whitening guide |
| 5692900, | Jun 07 1995 | Ultradent Products, Inc. | Patient dentist whitening guide |
| 5700148, | Mar 21 1995 | Ultradent Products? Inc.; ULTRADENT PRODUCTS, INCORPORATED | Syringe-deliverable neutralizing barrier |
| 5700478, | Aug 19 1994 | Ortho-McNeil Pharmaceutical, Inc | Water-soluble pressure-sensitive mucoadhesive and devices provided therewith for emplacement in a mucosa-lined body cavity |
| 5707235, | Apr 03 1995 | 3M Innovative Properties Company | Dental tray spacer |
| 5707736, | Apr 04 1991 | SION MICROTEC LTD | Products having anti-microbial activity |
| 5708052, | Apr 07 1995 | Ultradent Products, INC | Compositions and methods for priming and sealing dental and biological substrates |
| 5713738, | Dec 12 1995 | Discus Dental, LLC | Method for whitening teeth |
| 5722833, | Mar 21 1995 | Ultradent Products, INC | Viscous neutralizing barrier |
| 5723132, | Aug 23 1991 | GILLETTE COMPANY, THE | Sustained-release matrices for dental application |
| 5725843, | Mar 22 1990 | Ultradent Products, Inc. | Methods for bleaching teeth surfaces |
| 5730959, | Nov 14 1994 | Colgate Palmolive Company; Colgate-Palmolive Company | Storage stable aqueous dentifrice compositions having improved anticalculus properties |
| 5746598, | Mar 22 1990 | Ultradent Products, Inc. | Dental bleaching compositions including a sticky matrix material |
| 5759037, | Mar 22 1990 | Methods for manufacturing dental trays having thin walls for increased comfort | |
| 5759038, | Mar 22 1990 | Dental kit for applying sticky dental bleaching compositions to a person's teeth | |
| 5766011, | Nov 27 1996 | Dental bleaching composition and method | |
| 5770105, | Mar 22 1990 | Ultradent Products, Inc. | Methods for manufacturing sticky bleaching compositions |
| 5770182, | Mar 22 1990 | Ultradent Products, Inc. | Methods for treating teeth with anticariogenic and antimicrobial dental compositions |
| 5770219, | Sep 08 1989 | Ortho-McNeil Pharmaceutical, Inc | Solid matrix system for transdermal drug delivery |
| 5780045, | May 18 1992 | Minnesota Mining and Manufacturing Company | Transmucosal drug delivery device |
| 5785955, | Feb 23 1995 | Hemostatic compositions for treating soft tissue | |
| 5788579, | Jan 14 1997 | Illusion mirror light display | |
| 5789465, | Jul 27 1994 | KCI USA, INC | Composite surgical material |
| 5800832, | Oct 18 1996 | ARIUS TWO, INC | Bioerodable film for delivery of pharmaceutical compounds to mucosal surfaces |
| 5816804, | Jan 19 1996 | Ultradent Products, Inc. | Fiber-ended open orifice delivery tip |
| 5819765, | May 11 1994 | Finger glove comprising areas prepared for oral hygiene | |
| 5820854, | Mar 27 1997 | The Procter & Gamble Company; Procter & Gamble Company, The | Oral compositions containing polyoxyethylene |
| 5827525, | Sep 12 1995 | Bristol-Myers Squibb Company | Buccal delivery system for therapeutic agents |
| 5827591, | Oct 08 1996 | TRICOR DIRECT, INC | Removable adhesive notes for an industrial setting |
| 5846058, | Mar 22 1990 | Ultradent Products, Inc. | Dental trays having thin walls for increased patient comfort |
| 5851512, | Mar 22 1990 | Ultradent Products, Inc.; Ultradent Products, INC | Dental compositions having a sticky matrix material for treating sensitive teeth |
| 5851551, | Aug 23 1991 | GILLETTE COMPANY, THE | Sustained-release matrices for dental application |
| 5855870, | Mar 22 1990 | Ultradent Products, Inc.; Ultradent Products, INC | Method for treating sensitive teeth |
| 5858332, | Jan 10 1997 | Ultradent Products, Inc.; Ultradent Products, INC | Dental bleaching compositions with high concentrations of hydrogen peroxide |
| 5860809, | Aug 04 1997 | Lipstick display and device | |
| 5863202, | Nov 24 1992 | OROSCIENCE, INC | Device and method for treatment of dentition |
| 5871607, | Jan 10 1996 | The Procter & Gamble Company | Material having a substance protected by deformable standoffs and method of making |
| 5879591, | May 24 1995 | Tokuyama Corporation | Process for production of photochromic cured product |
| 5879691, | Jun 06 1997 | Procter & Gamble Company, The | Delivery system for a tooth whitener using a strip of material having low flexural stiffness |
| 5888480, | Jan 17 1995 | ProVSeal LLC | Methods, compositions, and dental delivery systems for the protection of the surfaces of teeth |
| 5891453, | Jun 06 1997 | The Procter & Gamble Company; Procter & Gamble Company, The | Delivery system for a tooth whitener using a strip of material having low flexural stiffness |
| 5894017, | Jun 06 1997 | Procter & Gamble Company, The | Delivery system for an oral care substance using a strip of material having low flexural stiffness |
| 5922307, | Sep 25 1995 | Discus Dental, LLC | Tooth bleaching compositions |
| 5953885, | Apr 08 1997 | AKI, INC | Cosmetic sampler and method of making using bulk thin film application techniques |
| 5965235, | Nov 08 1996 | The Procter & Gamble Co. | Three-dimensional, amorphous-patterned, nesting-resistant sheet materials and method and apparatus for making same |
| 5968633, | Jun 06 1997 | The Procter & Gamble Company; Procter & Gamble Company, The | Selectively-activatible sheet material for dispensing and dispersing a substance onto a target surface |
| 5980249, | Nov 24 1992 | OROSCIENCE, INC | Method and device for treatment of dentition |
| 5980868, | Jan 17 1995 | ProVSeal LLC | Methods, compositions, and dental delivery systems for the protection of the surfaces of teeth |
| 5985249, | Mar 22 1990 | Ultradent Products, INC | Sticky dental compositions for adhering a passive-type dental tray over a person's teeth |
| 5989569, | Jun 06 1997 | Procter & Gamble Company | Delivery system for a tooth whitener using a permanently deformable strip of material |
| 6030222, | Dec 01 1998 | MBKV LLC | Dye compositions and methods for whitening teeth using same |
| 6036943, | Mar 22 1990 | Ultradent Products, INC | Methods for treating a person's teeth using sticky dental compositions in combination with passive-type dental trays |
| 6045811, | Jun 06 1997 | Procter & Gamble Company, The | Delivery system for an oral care substance using a permanently deformable strip of material |
| 6083421, | Jan 19 1996 | IVOCLAR VIVADENT, INC | Film coating composition for whitening teeth |
| 6086855, | Mar 22 1990 | Ultradent Products, Inc. | Methods for making scalloped dental trays for use in treating teeth with sticky dental compositions |
| 6094889, | Feb 25 1997 | Exxon Chemical Patents, Inc. | Method of form and seal packaging |
| 6096328, | Mar 17 1998 | Procter & Gamble Company, The | Delivery system for an oral care substance using a strip of material having low flexural stiffness |
| 6099940, | Jul 16 1997 | The Procter & Gamble Company; Procter & Gamble Company, The | Selectively-activatible three-dimensional sheet material having multi-stage progressive activation to deliver a substance to a target surface |
| 6106293, | Dec 04 1998 | The Procter & Gamble Company | Methods for whitening teeth |
| 6126443, | Aug 13 1998 | 3M Innovative Properties Company | Medication delivery tray |
| 6136297, | Jun 06 1997 | Procter & Gamble Company, The | Delivery system for an oral care substance using a strip of material having low flexural stiffness |
| 6142780, | Feb 01 1999 | 3M Innovative Properties Company | Custom tray for delivering medication to oral structures |
| 6155825, | Jul 19 1999 | GUILFORD PHARMACEUTICALS, INC | Radiopaque endodontic marking tools and related methods |
| 6155832, | Dec 04 1998 | The Procter & Gamble Company | Methods and apparatus for whitening teeth |
| 6182420, | Apr 08 1997 | WILMINGTON TRUST, NATIONAL ASSOCIATION, AS THE SUCCESSOR COLLATERAL AGENT; ACQUIOM AGENCY SERVICES LLC, AS THE SUCCESSOR COLLATERAL AGENT | Method of making a cosmetic sampler using bulk thin film application techniques |
| 6183251, | Mar 22 1990 | Ultradent Products, Inc. | Scalloped dental trays for use in treating teeth with sticky dental compositions |
| 6194062, | Jan 10 1996 | The Procter & Gamble Company | Storage wrap material |
| 6197331, | Jul 24 1997 | DEXCEL PHARMA TECHNOLOGIES LTD | Pharmaceutical oral patch for controlled release of pharmaceutical agents in the oral cavity |
| 6217335, | Jun 06 1996 | Ultradent Products, INC | Endodontic systems and methods for the anatomicall, sectional and progressive corono-apical preparation of root canals with minimal apical intrusion |
| 6234793, | Jul 19 1999 | Ultradent Products, Inc.; Ultradent Products, INC | Textured dental matrix bands and related methods |
| 6254965, | Nov 08 1996 | The Procter & Gamble Company | Three-dimensional nesting-resistant sheet materials and method and apparatus for making |
| 6274122, | Jan 07 1999 | Device and method using dry mixtures for whitening teeth | |
| 6277458, | Mar 15 1999 | Procter & Gamble Company, The | Release strip with partible break to facilitate |
| 6287120, | Oct 08 1999 | The Procter & Gamble Company | Methods and apparatus for treating teeth |
| 6306206, | Jan 06 2000 | Ultradent Products, Inc. | Temporary dental cement compositions and related methods and systems |
| 6306370, | May 30 1997 | Ultradent Products, Inc. | Compositions and methods for whitening and desensitizing teeth |
| 6309625, | Nov 12 1998 | Ultradent Products, Inc. | One-part dental compositions and methods for bleaching and desensitizing teeth |
| 6322360, | Oct 22 1999 | 3M Innovative Properties Company | Medication retention assembly for oral delivery tray |
| 6343932, | Nov 13 2000 | The Procter & Gamble Company | Delivery system for whitening teeth |
| 6361844, | Jan 27 1999 | 3M Innovative Properties Company | Release article and adhesive article comprising the release article |
| 6368576, | Nov 12 1998 | Ultradent Products, Inc. | Methods for bleaching, opacifying and desensitizing teeth |
| 6379155, | Jun 06 1996 | Ultradent Products, INC | Endodontic systems and methods for the anatomical, sectional and progressive corono-apical preparation of root canals with instruments utilizing stops |
| 6391283, | Jan 10 1997 | Ultradent Products, Inc. | Methods and apparatus for activating dental compositions |
| 6400801, | Jul 19 1999 | Ultradent Products, Inc. | Smooth radiopaque endodontic marking tools and related methods |
| 6402514, | Mar 19 2001 | Ultradent Products, Inc. | Dental wedge with elastomeric sides for enhanced retention |
| 6461158, | Aug 14 2000 | Procter & Gamble Company, The | Products and methods that simulate changes in tooth color |
| 6468079, | Jul 19 1999 | Ultradent Products, Inc. | Abrasive radiopaque endodontic marking tools and related methods |
| 6500004, | Dec 14 2000 | Ultradent Products, INC | Endodontic sealing compositions and methods for using such compositions |
| 6514483, | Mar 12 2001 | Colgate Palmolive Company; Colgate-Palmolive Company | Strip for whitening tooth surfaces |
| 6527751, | Dec 20 1999 | Ultradent Products, INC | Hydraulic syringe and method of manufacture |
| 6551579, | Jun 06 1997 | Procter & Gamble Company, The | Delivery systems for a tooth whitener |
| 6582708, | Jun 28 2000 | Procter & Gamble Company, The | Tooth whitening substance |
| 6625839, | Jan 18 2000 | Ultradent Products, Inc. | Flocked tongue cleaning device |
| 6649147, | Jul 02 1999 | Procter & Gamble Company, The | Delivery system for oral care compositions comprising organosiloxane resins using a removable backing strip |
| 6652282, | Dec 14 2000 | Ultradent Products, Inc. | Endodontic sealing compositions and methods for using such compositions |
| 6729879, | Mar 13 2002 | Ultradent Products, INC | Dental bonding methods for adhering amalgam restoratives to dental substrates |
| 6746664, | Aug 06 2001 | Ultradent Products, Inc. | Multi-part dental bleaching systems and methods for bleaching teeth using such systems |
| 6756417, | Mar 13 2002 | Ultradent Products, INC | Dental bonding compositions for adhering amalgam restoratives to dental substrates |
| 6814794, | Nov 06 2002 | Ultradent Products, Inc. | Temporary dental cements having reduced tooth sensitivity |
| 6860736, | May 23 2003 | Ultradent Products, Inc.; Ultradent Products, INC | Oral treatment devices that include a thin, flexible barrier layer and an endoskeleton treatment or adhesive composition |
| 6884426, | Jun 06 1997 | The Procter & Gamble Co. | Methods for whitening teeth |
| 6916463, | Sep 24 2002 | Procter & Gamble Company, The | Oral products having an aesthetic layer |
| 6949240, | May 23 2002 | Procter & Gamble Company, The | Tooth whitening products |
| 6981874, | Oct 22 2003 | Ultradent Products, Inc.; Ultradent Products, INC | Dental bleaching compositions and devices having a solid activation adhesive layer or region and bleaching gel layer or region |
| 6994546, | Dec 18 2002 | Ultradent Products, Inc. | Light curing device with detachable power supply |
| 6997706, | Mar 04 2004 | Ultradent Products, Inc. | Fluoride-releasing pellet kit |
| 6997708, | Oct 22 2003 | Ultradent Products, Inc. | Treatment compositions and strips having a solid adhesive layer and treatment gel adjacent thereto |
| 7011523, | Oct 22 2003 | Ultradent Products, Inc.; Ultradent Products, INC | Bleaching compositions and devices having a solid adhesive layer and bleaching gel adjacent thereto |
| 7018622, | Jun 06 1997 | The Procter & Gamble Company | Structures and compositions increasing the stability of peroxide actives |
| 7040893, | Oct 30 2000 | Ultradent Products, INC | Fiber-covered dental delivery instruments |
| 7040897, | May 23 2003 | Ultradent Products, Inc. | Thin, flexible membrane dental trays and systems and methods utilizing such trays |
| 7048543, | May 27 2003 | Ultradent Products, Inc.; Ultradent Products, INC | Substantially solid bleaching composition in a tray-like configuration |
| 7052275, | May 27 2003 | Ultradent Products, Inc. | Kits and methods for bleaching and desensitizing teeth |
| 7056118, | May 27 2003 | Ultradent Products, Inc. | Compositions and devices having a tray-like configuration for delivering a medicament and methods of manufacturing and using such compositions and devices |
| 7059857, | May 27 2003 | Ultradent Products, Inc. | Substantially solid desensitizing compositions and devices having a tray-like configuration and methods of manufacturing and using such compositions and devices |
| 7059858, | Feb 19 2004 | Ultradent Products, Inc.; Ultradent Products, INC; ULTRADENT PRODUCTS, INC , | Universal tray design having anatomical features to enhance fit |
| 7074042, | May 27 2003 | Ultradent Products, Inc.; Ultradent Products, INC | Tray-like dental bleaching devices having a barrier layer and a substantially solid bleaching composition |
| 7094393, | Sep 25 1995 | Discus Dental, LLC | Tooth bleaching compositions |
| 7097449, | Mar 04 2004 | Ultradent Products, Inc. | Dental brackets for retaining a medicament-releasing pellet on a tooth and kits including such brackets |
| 7121828, | Jun 09 2004 | Ultradent Products, Inc. | Reinforced gingival retraction cord |
| 7122199, | Jun 06 1997 | Procter & Gamble Company, The | Methods for whitening teeth |
| 7128899, | Jan 27 2001 | Ultradent Products, Inc. | Bleaching device comprising a barrier layer and a bleaching composition comprising polyvinylpyrrolidone |
| 7144250, | Dec 17 2003 | Ultradent Products, Inc.; Ultradent Products, INC | Rechargeable dental curing light |
| 7168951, | Jun 09 2004 | Ultradent Products, Inc. | Reinforced gingival retraction cord |
| 7172423, | May 27 2003 | Ultradent Products, Inc. | Substantially solid bleaching or treatment compositions in the form of inserts for dental trays, and kits comprising such inserts and trays |
| 7192276, | Aug 20 2003 | Ultradent Products, Inc. | Dental curing light adapted to emit light at a desired angle |
| 7192280, | Feb 19 2004 | Ultradent Products, Inc. | Dental bleaching devices having a protective adhesive region |
| 7198619, | Mar 26 2002 | Ultradent Products, Inc.; Ultradent Products, INC | Valve syringe |
| 7198623, | Jan 10 2003 | Ultradent Products, INC | Fiber-coated dental infusor systems and methods of use |
| 7264471, | May 05 2004 | Ultradent Products, Inc. | Methods and kits for bleaching teeth while protecting adjacent gingival tissue |
| 7320598, | Dec 14 2000 | Ultradent Products, Inc. | Method for filling and sealing a root canal |
| 7398598, | May 13 2003 | Ultradent Products, Inc.; Ultradent Products, INC | Methods for manufacturing endodontic instruments |
| 7534264, | Jan 28 2004 | Ultradent Products, Inc. | Delivery system for bone growth promoting material |
| 7780449, | Apr 23 2002 | Ultradent Products, Inc. | Hydrophilic endodontic sealing compositions and methods for using such compositions |
| 7862801, | Jan 27 2001 | Ultradent Products, Inc. | Adhesive dental bleaching compositions comprising polyvinylpyrrolidone |
| 7862802, | Mar 17 2000 | LG HOUSEHOLD & HEALTH CARE LTD. | Patches for teeth whitening |
| 8524200, | Sep 11 2002 | The Procter & Gamble Company | Tooth whitening products |
| 20010009755, | |||
| 20020006387, | |||
| 20020018754, | |||
| 20020146666, | |||
| 20030145863, | |||
| 20030147258, | |||
| 20030148242, | |||
| 20030156980, | |||
| 20030199605, | |||
| 20030211056, | |||
| 20030215766, | |||
| 20040120903, | |||
| 20040122377, | |||
| 20040214130, | |||
| 20040214131, | |||
| 20040214140, | |||
| 20040249016, | |||
| 20050016884, | |||
| 20050019277, | |||
| 20050064371, | |||
| 20050069837, | |||
| 20050130096, | |||
| 20050136373, | |||
| 20050238591, | |||
| 20050249680, | |||
| 20050287086, | |||
| 20070003495, | |||
| 20070086961, | |||
| CA1209761, | |||
| CA2000040, | |||
| CA2078960, | |||
| CA2095445, | |||
| CA681997, | |||
| DE1104116, | |||
| DE2330869, | |||
| EP252459, | |||
| EP328317, | |||
| EP637446, | |||
| FR2637175, | |||
| FR2701397, | |||
| GB1240411, | |||
| GB2108841, | |||
| GB2115431, | |||
| GB2159052, | |||
| IE42604, | |||
| JP10017448, | |||
| JP10040423, | |||
| JP10226639, | |||
| JP1279838, | |||
| JP2202814, | |||
| JP2250826, | |||
| JP3198754, | |||
| JP3264522, | |||
| JP3264523, | |||
| JP5124954, | |||
| JP5220203, | |||
| JP5236885, | |||
| JP57028102, | |||
| JP58213709, | |||
| JP60005159, | |||
| JP60005160, | |||
| JP61280423, | |||
| JP62142113, | |||
| JP62255417, | |||
| JP63005756, | |||
| JP63054318, | |||
| JP6321744, | |||
| JP7100186, | |||
| JP8183732, | |||
| JP8325128, | |||
| RE33093, | Nov 16 1988 | Johnson & Johnson Consumer Products, Inc. | Bioadhesive extruded film for intra-oral drug delivery and process |
| RE34196, | Aug 23 1988 | DUNHALL PHARMACEUTICALS, INC | Method and material for brightening teeth |
| RU2075965, | |||
| WO198806879, | |||
| WO198910740, | |||
| WO199106289, | |||
| WO199116041, | |||
| WO199517158, | |||
| WO199625910, | |||
| WO199817263, | |||
| WO199855044, | |||
| WO1999027895, | |||
| WO2003015656, | |||
| WO2005058266, |
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